Precursors Part 1

acetaldehyde CH₃CHO CAS number 75-07-0

mp -123.5 bp 21 d 0.788 m 44.05 c $?.??

Safety Data: MSDS Flammable table key

Synonyms: acetic aldehyde; acetylaldehyde; aldehyde; ethanal; ethyl aldehyde; ethylaldehyde
Synthesis:    Place 260 mL of 23% sulfuric acid in a 1500-mL Florence flask. Connect an addition funnel to the flask, and set it up for vacuum distillation with a 500-mL receiving flask. The receiving flask should be immersed in a salt-ice bath to cool the distillate when it comes over. Although a setup for vacuum distillation is used, it is not necessary to apply a vacuum; the vacuum adapter merely provides a means of equalizing pressure. Prepare a solution of 100 g of sodium dichromate in 200 mL of water and 127 mL of ethyl alcohol. Factor in the amount of water that is already in the ethyl alcohol when making the solution, i.e. 100 mL of 95% alcohol has 5 mL of water in it already. Place this solution in the addition funnel, position the stem of the funnel such that it is about 3 cm above the surface of the acid. Heat the acid until it just begins to boil, then add the mixture in the funnel in a steady stream to the acid. It will not be necessary to heat the flask during the addition because it will generate its own heat. The heat will be sufficient to distill over the acetaldehyde along with some alcohol and waste acetal. If acetaldehyde vapors begin to escape from the flask, regulate the distillation by decreasing the amount of dichromate solution being added. If the reaction flask does not boil on its own, gently heat it for a short time until boiling begins.
     The crude acetaldehyde thus obtained is difficult to distill from the alcohol and acetal mixed with it. It is therefore converted to aldehyde-ammonia, then back to pure aldehyde. Place the crude acetaldehyde in a Florence flask of suitable volume to contain no more than two thirds of the liquid. Attach a reflux condenser to the flask. Fill the condenser jacket with 30 °C water. It is only necessary to have the warm water in the jacket, not flowing. Stop up the lower connecter to prevent water from leaking out. To the top of the condenser, attach a glass tube connected to a wash bottle filled with 50 mL of ethyl ether. This wash bottle is then connected to another wash bottle filled with 50 mL of ether. After all connections have been made, the crude aldehyde is heated to a gentle boil for 5-10 minutes. The ether will absorb the acetaldehyde as it boils off. If the ether begins to rise up into the connecting tube from the condenser to the wash bottle, increase the heating. Combine the ether into a 150-mL beaker immersed in a salt-ice bath. Bubble dry ammonia gas into the ether through an inverted funnel or wide tube immersed near the bottom of the beaker. Add ammonia until the ethereal solution smells strongly of ammonia. After about an hour, pure ammonia-aldehyde should have separated out. Scrape the crystals from the beaker and collect them by suction filtration. Wash the crystals with a small amount of ether, and allow them to dry in a desiccator. The yield is about 30 g.
     To obtain pure acetaldehyde, dissolve 10 g of aldehyde-ammonia in 10 mL of water in a 50-mL Florence flask. Add 28 mL of cold 29% sulfuric acid to the flask and set it up for simple distillation. Heat the flask on a water bath to distill over the aldehyde. Place the receiving flask in a salt-ice bath to cool the volatile acetaldehyde.
     Acetaldehyde is extremely volatile and cannot be stored satisfactorily unless it is refrigerated or sealed in glass ampoules (not just capped), therefore it is necessary to prepare acetaldehyde each time it is needed. There is, however, an easier solution. A quick and easy way to store acetaldehyde is to polymerize it to paraldehyde, which can be handled and stored easily, then depolymerize when you need to use it. Now you can make a larger amount without worry.
     To polymerize acetaldehyde for storage, place it in a dry test tube and cautiously add 1 drop of concentrated sulfuric acid per 2 mL of acetaldehyde in the tube. Mix thoroughly, the polymerization will begin to take place. Some gentle warming can hasten the reaction. After some minutes add 3-4 mL of water per 2 mL of acetaldehyde, an insoluble precipitate of paraldehyde will form. As an aside, technically paraldehyde is a controlled substance. It is a sedative and a hypnotic drug useable by prescription only.
     To depolymerize paraldehyde back into acetaldehyde, place the paraldehyde into a round-bottom 200-mL Florence flask. Add 4-5 drops of concentrated sulfuric acid for every 20 g (20 mL) of paraldehyde in the flask. Set the flask up for fractional distillation, use glass in the fractionating column. Use a 125-mL Erlenmeyer flask as the receiver; keep it cool by immersing in an ice water (but not salt-ice) bath. Place a loose plug of cotton into the Erlenmeyer flask to help reduce evaporation loss; it must be loose. Care must be taken to prevent the cotton from coming into contact with the distillate. After setting up, heat the flask gently. The temperature of the distillate must not be allowed to rise above 35 °C as it will only repolymerize. The acetaldehyde is now ready for use.

acetamide CH₃CONH₂ CAS number 60-35-5

mp 81 bp 222 d 1.159 m 59.07 c $?.??

Safety Data: MSDS

Synonyms: acetic acid amide; acetimidic acid; ethanamide; methanecarboxamide
Synthesis:    Place 71.5 mL of glacial acetic acid into a ceramic or porcelain dish, heat the acid to 40-50 °C by a water bath. Neutralize the acid by adding 100 g of finely pulverized ammonium carbonate; the resulting compound should be slightly alkaline. The mass is warmed on the water bath to 80-90 °C until acidic, test for acidity by adding a few drops to a test tube of water then drop on litmus or pH paper.
     The reaction is now completed in a bomb tube, or Volhard tube, this is essentially a glass bottle that is sealed by melting the glass together at the opening. Since these may be hard to come by a substitute is needed. A heavy walled glass beer or wine bottle should lend itself well to acting as a reaction container. There is a strong possibility that such a bottle can burst under the great heat required of this reaction, this applies to the Volhard tube as well. The tube or bottle should be wrapped in a fine mesh metal screen, the kind used on windows, if it bursts the screen will prevent glass going everywhere. Heating the tube behind a sheet of wood is also a good idea.
     It will be quite necessary to melt the top of the glass closed; using a mere rubber or cork stopper is not sufficient because they will melt or burn. To seal the open end of a tube charged with the substance, it is warmed by holding it at an angle of about 45°, with constant turning, in the small luminous flame of a burner, and then heated strongly in the larger non-luminous flame. Heat the neck if using a bottle. When the glass becomes soft, use pliers to gently pull and squeeze the top of the tube upwards causing the glass of the neck to narrow. Continue to heat this narrowed portion and draw the top up until the glass has closed itself off. After breaking off or cutting of the end of the tip, to allow the air to escape on further heating, it is heated just below the top. When the tube is softened at this point it is drawn out slightly, heat is applied just below the top, it is drawn out again, and so on. The result is that the form of the top of the tube gradually changes from a cylinder to a sharp-pointed cone. The narrowest part of the cone is then heated without drawing it further. The soft glass melts together, and a thick walled cap is obtained.
     Fill the tube, previously heated by flame, with the compound while hot without using a funnel. If any portion adheres to the top of the tube, melt it down by carefully heating with a flame. Any remaining trace can be wiped away, now seal the tube as described above. Heat the tube for 5 hours at 220-230 °C in a furnace. After heating, break the bottle open to obtain the reaction product. The liquid product is fractionally distilled in a well ventilated area. The first fraction that distills over between 100-130 °C will be acetic acid and water. The temperature will then rise rapidly to 180 °C where upon acetamide will begin to distill over. Collect the portion distilling over between 180-230 °C in a beaker. Cool the beaker with a salt-ice bath towards the end of the distillation. Rub the walls of the beaker after the distillation to crystallize the impure acetamide. The crystals are placed on a Buchner funnel and pressed to squeeze out any liquids. The crystals are now simple distilled to obtain almost pure acetamide. To remove the last traces of impurities, again press the crystals, then recrystallize from a minimum amount of ethyl ether. Filter to collect the crystals, allow a brief period to dry. Yield is about 40 g.

acetic acid CH₃COOH CAS number 64-19-7

mp 16.7 bp 118 d 1.0492 m 60.05 c $?.??

Safety Data: MSDS Corrosive, Flammable

Synonyms: acetate; acetic acid glacial; Aci-Jel; ethanoic acid; ethylic acid; glacial acetic acid; methanecarboxylic acid; shotgun; TCLP extraction fluid 2; vinegar; vinegar acid
Synthesis: Acetic acid is available as an OTC chemical in the form of vinegar, a dilute solution of acetic acid. Vinegar should be available from any grocery story in 3%-5% concentrations or so. Acetic acid is a chemical that I consider to plentiful to bother synthesizing yourself since it is a cheap, abundant OTC chemical. It can be done, and it may be cheaper in the long run to make it on your own, but I do not have the information handy. A trip to the library, or a web search will yield much info on the topic. Acetic acid is more useful in concentrated, or glacial, form. Only acetic acid is referred to as glacial rather than concentrated acid. This is because the ancients liked how much frozen acetic acid looked, it reminded them of an ice glacier, so the term glacial stuck. Glacial acetic acid is very corrosive and slightly flammable.
Vinegar can be made into glacial acetic acid by first converting it to sodium acetate. Once you have some sodium acetate ready, set up the necessary equipment for a simple distillation and fill the reaction flask with concentrated (95%+) sulfuric acid. Add the sodium acetate to the acid and begin the distillation. The sulfuric acid will break down the sodium acetate and the resulting acetic acid will distill off. The concentration of the acetic acid obtained will be nearly anhydrous, especially if you start with thoroughly dried sodium acetate and 100% sulfuric acid.

acetic anhydride (CH₃CO)₂O CAS number 108-24-7

mp -73 bp 139 d 1.080 m 102.09 c $?.??

Safety Data: MSDS Corrosive, Flammable

Synonyms: acetic acid anhydride; acetic oxide; acetyl anhydride; acetyl ether; acetyl oxide; ethanoic anhydrate; ethanoic anhydride
Synthesis: Acetic anhydride is a very handy organic compound that has fallen into ill repute thanks to the drug dealers. It is technically a watched chemical, but you will only have to answer questions at gunpoint if you buy over 250 gallons. Even so, you will most likely be put on The List if you buy any, and you will have to come up with a bunch of explanations as to what you are going to do with it. Acetic anhydride is very corrosive and must be kept away from moisture, as it will decompose into acetic acid.
Into a 200-mL Florence flask, add 70 g of finely pulverized, anhydrous sodium acetate. Set the flask up for simple distillation, instead of a thermometer in the top of the flask use an addition funnel. Slowly add, by dropwise addition, 45.5 mL of acetyl chloride from the addition funnel. After half of the acetyl chloride has been added, stop the addition and stir the reaction mix with a glass stirring rod. Afterwards, continue the addition the rest of the way. If at any point during the addition some material should distill over, pour it back into the reaction flask and decrease the rate of addition to prevent this. After the addition is complete, remove the addition funnel, stop up the flask, and distill with flame or hot plate. The crude acetic anhydride thus obtained needs to be purified by distillation. Set up for a simple distillation, add 3 g of finely pulverized, anhydrous sodium acetate to the reaction flask, and then pour in the crude acetic anhydride. The sodium acetate will convert any remaining acetyl chloride into the anhydride. The receiving flask should be under a water shower for cooling. Place a large funnel (a cheap plastic one will work fine) under the flask with a tube leading to the sink, pour cold water over the top of the receiving flask. The receiving flask can also be held directly under the faucet in the sink. Commence the distillation; the yield should be about 50 g of pure acetic anhydride.

acetone CH₃COCH₃ CAS number 67-64-1

mp -94 bp 56.5 d 0.788 m 58.08 c $?.??

Safety Data: MSDS Flammable

Synonyms: 2-propanone; chevron acetone; dimethyl formaldehyde; dimethylketal; dimethyl ketone; ketone propane; beta-ketopropane; methyl ketone; propanone; pyroacetic acid; pyroacetic ether
Synthesis: Acetone is available as an OTC chemical in just about every hardware store. The stores sell it cheap, pure, and in large quantities. As far as Synthesis goes it is rather complicated, so it is best to purchase it. Its primary use in the household is as a solvent for paint, i.e. thinning paint, removing varnishes, and cleaning brushes. It can be purchased in pint to 5-gallon sizes at hardware stores or paint supply stores without question.
Acetone can be dried out by adding a small amount of calcium chloride, say 1 g per 25 mL, and letting it stand for three to seven days in a sealed container. Occasional agitation, every 12-24 hours, will improve the drying process. After letting the acetone stand, distill it to get the dry acetone. Some of the acetone will combine with the calcium chloride, so it necessary to distill it. Store the dry acetone in a well-sealed container.

acetyl chloride CH₃COCl CAS number 75-36-5

mp -112 bp 52 d 1.104 m 78.50 c $?.??

Safety Data: MSDS

Synonyms: acetic acid chloride; acetic chloride; ethanoyl chloride
Synthesis: Place 95 mL of glacial acetic acid into a round-bottomed 500-mL Florence flask. Set the flask up for vacuum distillation with addition. Instead of connecting the vacuum adapter to a vacuum source, attach a calcium chloride drying tube. There is no need for vacuum, just an airtight connection to protect the product from moisture. While cooling the flask in a salt-ice bath, slowly add 51 mL of phosphorus trichloride through the addition funnel. After the addition, place the flask in a water bath heated to 40-50 °C. Continue heating until the active evolution of hydrochloric acid gas slackens, and the liquid separates into two layers.
To separate the acetyl chloride, which should have formed on the upper layer, heat the flask on a boiling water bath until nothing more distills over. To purify the acetyl chloride, simple distill the product obtained in the same apparatus used before, except this time replace the addition funnel with a thermometer. Collect the portion distilling over from 50 to 56 °C. The yield is about 80-90 g.

acrylic acid CH₂=CHCO₂H CAS number 79-10-7

mp 14 bp 141.0 d 1.0621 m 72.06 c $?.??

Safety Data: MSDS Corrosive, Flammable

Synonyms: 2-propenoic acid; acroleic acid; acrylate; ethylenecarboxylic acid; propene acid; propenoic acid; vinylformic acid
Synthesis:    Prepare a mixture of 151 mL of 98-100% formic acid, 1060 mL of methyl acrylate, 30 g of hydroquinone, and 2 mL of sulfuric acid in a round-bottomed 2-L flask. Set the flask up for refluxing. Reflux with an oil bath heated to 85-95 °C (the oil not the contents of the flask) for 1-3 hours.
     Remove the reflux column and set the flask up for fractional distillation, using copper sponge to pack the column. Slowly distill the mixture at 32-35 °C for about 8-10 hours, you will be removing methyl formate waste from the mixture. You will want to let 1 drop of distillate come over for every 5 that fall back into the flask, then allow more to come over near the end.
     When no more methyl formate is produced, the excess methyl acrylate is fractionally distilled under partial vacuum at 32-35 °C with the oil temperature at 60-65 °:C. Reconfigure the setup for vacuum distillation if need be. You will also need to add a clasien adapter so as to extend a length of tubing into the mixture. During the distillation, a slow stream of carbon dioxide is admitted through this tube.
     When all the methyl acrylate has been removed, the acrylic acid is fractionally distilled at 53-56 °C under vacuum. Upon redistillation acrylic acid of 97% purity is obtained in a yield of 74-78% or about 220-230 g.

acrylyl chloride H₂C=CHCOCl CAS number 814-68-6

mp ? bp 72-76 d 1.1140 m 90.51 c $?.??

Safety Data: MSDS Corrosive, Flammable

Synonyms: acryl chloride; acrylic acid chloride; acryloyl chloride; chlorid kyseliny akrylove; 2-propenoyl chloride; propenoyl chloride
Synthesis: Into a 1-L round-bottomed flask place 135 mL of thionyl chloride. Set this flask up for refluxing with addition. Heat the thionyl chloride to boiling, and then add 115 mL of acrylic acid at such a rate that the mixture refluxes gently. It may require about an hour to add all of the acid. This reaction will generate toxic sulfur dioxide gas, so take the necessary precautions. After all of the acid has been added, continue to reflux for an additional 30 minutes to expel all of the sulfur dioxide gas.
I have no information on how to isolate or purify this chemical. It will be mixed with hydrochloric acid as a waste byproduct. I would suggest neutralizing the acid by adding some sodium hydroxide, and then distilling the product to get pure acrylyl chloride. If using this chemical to make 1,1,1-trinitro-2-propyl acrylate, try using aluminum hydroxide to neutralize the acid. The product of this is aluminum chloride, which is needed in the reaction, so no need to distill this.

allyl methanesulfonate C₄H₈O₃S CAS number 6728-21-8

mp ? bp ? d ? m 136.1 c $?.??

Safety Data: MSDS

Synonyms: allyl mesylate; methanesulfonic acid, allyl ester; methanesulfonic acid, 2-propenyl ester
Synthesis: In a 1000-mL Erlenmeyer flask prepare a solution of 20 g of distilled allyl alcohol (98%) in 300 mL of diethyl ether. Cool the flask in an ice-water bath to below 5 degrees C. With stirring add 56.5 g of solid potassium carbonate in one portion; next add 3.3 g of solid trimethylamine hydrochloride in one portion. Stir the resulting suspension for 5 minutes. With vigorous stirring add 46.9 g of methanesulfonyl chloride to the flask dropwise over a period of 1 hour. After the addition of methanesulfonyl chloride is complete continue stirring the contents of the flask for 5 hours and maintain the temperature at 5 degrees C. Next add 300 mL of water to the flask and continue to stir the contents vigorously for an additional 15 minutes before discontinuing the stirring. Allow the contents of the flask to separate into two layers, the aqueous layer will be on the bottom. Decant off as much of the aqueous layer as possible by a pipette and collect it in a separate beaker. Mix the aqueous portion with two portions of 100 mL of ethyl ether and shake them in a seperatory funnel. It may be necessary to break up the aqueous layer into four batches to fit into the seperatory funnel, in which case shake each 75 mL portion of water with two 25 mL portions of ether. Combine all of the ether extracts with the organic layer in an Erlenmeyer flask and add a portion of anhydrous magnesium sulfate to draw out any moisture. Remove the ether by evaporating under reduced pressure without heating. The remaining allyl methanesulfonate is poured over a filter to remove the magnesium sulfate and kept under high vacuum to remove any final traces of solvent. What remains should be about 38-39 g of clear colorless oil. Yield is 83%. If possible this reaction should be carried out under an atmosphere of nitrogen.

aluminum Al CAS number 7429-90-5

mp 660 bp 2327 d 2.70 m 26.981539 c $?.??

Safety Data: MSDS Flammable

Synonyms: aluminium
Synthesis:    Aluminum powder will add explosive strength to just about any high explosive. The powder only that is, not foil or wire. The kind of powder needed is very finely divided, not the kind that can be purchased from automotive stores as a leak plugger for the radiator, that variety is too coarse. The only possible OTC source is from paint stores as an additive for paint. I should mention that I have never seen it sold in paint stores.
     If all else fails one can buy finely powered aluminum from chemical suppliers who deal with the public. Companies that sell pyrotechnic materials will in all likelihood have several grades available from coarse down to atomized.
     When using aluminum in chemical reactions one can use aluminum foil available at any grocery store, or aluminum tubing or rod available at hardware stores. Aluminum products are quite abundant at many stores. Aluminum foil is quite versatile because it offers a higher surface area compared to other types of OTC aluminum, it is quite cheap, and is pure. Aluminum foil is easy to tear into a desired mass and can be crumpled into balls of any size if coarse bits are needed for a reaction. Aluminum tubing or rod will need to be machined to get turnings, chunks, or shot which sounds like a lot work and special equipment.

aluminum chloride AlCl₃ CAS number 7446-70-0

mp ? bp ? d ? m 133.34 c $?.??

Safety Data: MSDS Corrosive

Synonyms: AlCl3; alluminio(cloruro di); aluminiumchlorid; aluminium, (chlorure d'); aluminium trichloride; aluminum chloride (1:3); chlorure d'aluminium; Drysol; NSC 143016; PAC (salt); Pearsall; trichloroaluminum; UN 1726; UN 2581
Synthesis: The Synthesis of aluminum chloride will require a creative glassware setup. Assemble a heating apparatus as shown in the illustration below; each part must be completely dry for the reaction to work. The long furnace tube of hard glass should be 1.5 to 2 cm in diameter. The length is up to you, but a tube of 25-40 cm should suffice. One end of the tube can be drawn out to a narrow aperture if desired, since that requires some glassblowing skill it may be difficult for the improviser. A stopper with a short length of glass tubing in the middle will do nicely. The wide end of the tube is inserted into the center of a large stopper, a second glass tube, of at least 8 mm diameter, bent at a right angle, is placed above the larger. The large stopper is then attached to a wide mouth glass bottle. The part of the tube extending beyond the flames must be as short as possible to prevent the product from condensing prematurely, or it will clog the tube. Each end of the tube is plugged with glass wool to keep the reactants inside. A heat resistant plate is secured between the bottle and the flame to protect the stopper from burning or melting, you can use glass wool, aluminum foil, or any kind of fire resistant material (asbestos was recommended, it is now unavailable). If you have a stopper at the other end instead of a narrowed end, you will need a plate there too. Fill the glass tube half way (horizontally, not vertically) with aluminum shavings before assembling of course. You can use little aluminum foil balls, or machine shop shavings, the latter must be cleaned of oil by boiling in ethyl alcohol and dried in an oven at 120 °C.
A very rapid current of dry hydrogen chloride gas is passed into the tube from the narrow end; the gas first passes into two drying bottles filled with concentrated sulfuric acid. Do not fill the bottles with too much acid as it can foam up. Test to see if all of the air has been removed from the apparatus by connecting a rubber hose to the angled outlet tube and directing the gas into a beaker of water. When only HCl gas remains, it will be absorbed directly into the water with little or no bubbling, now remove the tubing. If any air remains, there can be an explosion of oxygen and hydrogen. Now that the air is out, begin heating the tube with several burners along its length. Start with small flames and gradually increase. White vapors of aluminum chloride will begin to be evolved when the flames are high enough, and will be condensed into the bottle. Do not heat the aluminum so high it melts, if this happens remove the flames immediately. Continue heating when it solidifies. The reaction is done when all of the aluminum has been consumed, a small amount of dark residue may remain. The current of hydrogen chloride gas must be kept constantly rapid for this reaction to work. The aluminum chloride thus obtained is quite pure; store it in tightly sealed bottles or a desiccator.

aminoguanidine bicarbonate C₂H₈N₄O₃ CAS number 2582-30-1

mp ? bp ? d ? m ? c $?.??

Safety Data: MSDS Irritant

Synonyms: aminoguanidinium hydrogen carbonate; carbonic acid with hydrazinecarboximidamide (1:1)
Synthesis:    Two hundred and sixteen grams (2.07 moles) of nitroguanidine1 and 740 g. (11.3 moles) of purified zinc dust (Note 1) are thoroughly ground together in a mortar, and then enough water (about 400 ml.) is added with stirring with the pestle to form a thick paste. The paste is transferred to a 3-l. enameled can or beaker surrounded by an ice bath. A solution of 128 g. (2.14 moles) of glacial acetic acid in 130 ml. of water is cooled to 5� in another 3-l. beaker, which is fitted with a strong mechanical stirrer and surrounded by an ice bath. The paste of nitroguanidine and zinc dust, cooled to 5�, is added slowly with mechanical stirring, the temperature of the reaction mixture being kept between 5� and 15�. A total of about 1 kg. of cracked ice is added to the mixture from time to time as the mixture becomes too warm or too thick to stir. The addition of the paste takes about 8 hours, and the final volume of the mixture is about 1.5 l. (Note 2). The mixture is then slowly warmed to 40� on a water bath with continued stirring, and this temperature is maintained for 1�5 minutes, until reduction is complete (Note 3).
     The solution is immediately separated from the insoluble material by filtration on a 20-cm. B�chner funnel, and the cake is sucked as dry as possible. The residue is transferred to the 3-l. beaker, triturated well with 1 l. of water, and then separated from the liquid by filtration. In the same manner, the residue is washed twice more with two 600-ml. portions of water. The filtrates are combined and placed in a 5-l. round-bottomed flask. Two hundred grams of ammonium chloride is added, and the solution is mechanically stirred until solution is complete (Note 4). The stirring is continued, and 220 g. (2.62 moles) of sodium bicarbonate is added during a period of about 10 minutes. The aminoguanidine bicarbonate begins to precipitate after a few minutes, and the solution is then placed in a refrigerator overnight. The precipitate is collected by filtration on a B�chner funnel. The cake is removed to a 1-l. beaker and mixed with a 400-ml. portion of a 5% solution of ammonium chloride and filtered. It is again washed with two 400-ml. portions of distilled water, the wash solution being removed each time by filtration. Finally the solid is pressed down on the B�chner funnel; the mat is broken up with a spatula and washed while on the funnel with two 400-ml. portions of 95% ethanol and then with one 400-ml. portion of ether. After air drying, the aminoguanidine bicarbonate amounts to 180�182 g. (63�64%) of a white solid, melting at 172� with decomposition (Note 5) and (Note 6).
     1. The zinc is purified by stirring 1.2 kg. of commercial zinc dust with 3 l. of 2% hydrochloric acid for 1 minute. The acid is removed by filtration, and the zinc is washed in a 4-l. beaker with one 3-l. portion of 2% hydrochloric acid, three 3-l. portions of distilled water, two 2-l. portions of 95% ethanol, and finally with one 2-l. portion of absolute ether, the wash solutions being removed each time by filtration. Then the material is thoroughly dried and any lumps are broken up in a mortar.
     2. The solution becomes basic to litmus after one-half to three-fourths of the paste has been added. Lower yields are obtained if a larger excess of acetic acid is employed.
     3. The state of reduction can be determined by placing 3 drops of the reaction mixture in a test tube containing 5 ml. of a 10% solution of sodium hydroxide and then adding 5 ml. of a freshly prepared saturated solution of ferrous ammonium sulfate. A red coloration indicates incomplete reduction; when the reduction is complete, only a greenish precipitate is observed. The mixture should not be heated after this test shows that reduction is complete.
     4. The presence of the ammonium chloride prevents the coprecipitation of zinc salts when sodium bicarbonate is added to the solution to precipitate the aminoguanidine as the bicarbonate. If the solution is not clear at this step, it should be filtered.
     5. The aminoguanidine bicarbonate is pure enough for most purposes. It should not be recrystallized from hot water, since decomposition will occur.
     6. W. W. Hartman and Ross Philips have submitted a procedure suitable for the preparation of aminoguanidine bicarbonate on a larger scale. The sulfates of methylisothiourea and of hydrazine are allowed to react with the evolution of methyl mercaptan. In a 30-gal. crock are placed 10 l. of water and 5760 g. (20 moles) of methylisothiourea sulfate.2 In a 22-l. flask, 5.2 kg. (40 moles) of hydrazine sulfate3 is stirred with 12 l. of water, and 40% sodium hydroxide is added until all the hydrazine sulfate has dissolved and the solution is just neutral to Congo paper. The exact amount of alkali is noted and a duplicate amount added. The hydrazine solution is then added to the 30-gal. crock with stirring, as fast as possible, without allowing the foam to overflow the crock. The mixing is done out-of-doors, or in an efficient hood, since large volumes of methyl mercaptan are evolved. If the reaction is carried out on a smaller scale in 12- or 22-l. flasks, using appropriate amounts of material, the methyl mercaptan evolved may be absorbed in cold sodium hydroxide solution and isolated if desired. The solution is stirred until evolution of mercaptan stops, and then a few liters of water are distilled off under reduced pressure to free the solution entirely from mercaptan. The residual liquor is chilled in a crock, and a crop of hydrated sodium sulfate is filtered off, washed with ice water, and discarded. The filtrate is warmed to 20�25�, 25 ml. of glacial acetic acid is added, then 4 kg. of sodium bicarbonate, and the solution is stirred vigorously for 5 minutes and thereafter occasionally during an hour, or until the precipitate no longer increases. The precipitate is filtered with suction and washed with ice water and then with methanol, and is dried at a temperature not above 60�70�. The yield is 3760 g. (69% of the theoretical amount). Hydrazine sulfate may be recovered from the final filtrate, if the filtrate is strongly acidified with sulfuric acid and allowed to cool.
This procedure borrowed from Organic Synthesis Collective Volume 3 pg 73

ammonia NH₃ CAS number 7664-41-7

mp -77.7 bp -33.35 d 0.6818 m 17.03 c $?.??

Safety Data: MSDS Corrosive, Irritant, Toxic

Synonyms: N-H
Synthesis: One method gaseous ammonia can be generated is by heating a small flask full of the most concentrated ammonium hydroxide available with a burner, household hydroxide will not be sufficient. The gas can be dried by passing it through a drying tube filled with a mixture of 4 parts calcium oxide with 1 part sodium hydroxide.

ammonium carbonate (NH₄)₂CO₃ CAS number 506-87-6

mp ? bp ? d ? m ? c $?.??

Safety Data: MSDS

Synonyms: ammonium sesquicarbonate; carbonic acid, ammonium salt; carbonic acid, diammonium salt; crystal ammonia; diammonium carbonate; hartshorn
Synthesis: Coming soon!

ammonium chloride NH₄Cl CAS number 12125-02-9

mp ? bp ? d 1.5274 m 53.49 c $?.??

Safety Data: MSDS

Synonyms: Amchlor; ammoneric; ammoniumchlorid; ammonium muriate; chlorid amonny; Darammon; sal ammonia; sal ammoniac; salammonite; salmiac
Synthesis: Coming soon!

ammonium ferrous sulfate (NH₄)₂Fe(SO₄)₂ � 6 H₂O CAS number 10045-89-3

mp 100 (dec) bp - d 1.86 m 284.05 c $?.??

Safety Data: MSDS

Synonyms: ammonium iron sulfate; ferrous ammonium sulfate; iron ammonium sulfate; Mohr's salt; sulfuric acid, ammonium iron(2+) salt
Synthesis: Prepare a solution of 234 g of ammonium bisulfate in 1 L of water. Add 42.7 g iron metal to the solution and heat to 70 degrees C until all of the iron dissolves (reacts). Add an additional 234 g of ammonium bisulfate to the solution and again add 42.7 g of iron and heat to 70 degrees until all of the iron reacts. Cool the solution down to less than 15 degrees C with stirring; ammonium ferrous sulfate should then precipitate. Pour the liquid over a filter to collect the crystals. You may need to boil the liquid down to half its volume to obtain a complete crop of crystals.
The ammonium bisulfate used in this reaction can be obtained by heating ammonium sulfate to 370 degrees C and cooking for about 15-20 minutes. Ammonium sulfate can be obtained either as fertilizer or by reacting ammonia with sulfuric acid.

ammonium hydroxide NH₄OH CAS number 1336-21-6

mp - bp - d 0.90 m - c $?.??

Safety Data: MSDS Corrosive

Synonyms: ammonia, monohydrate; ammonia water; ammonium, aqueous; aqua ammonia; aqueous ammonia; Spirit of Hartshorn
Synthesis: Coming soon!

aniline C₆H₅NH₂ CAS number 62-53-3

mp -6 bp 184-186 d 1.022 m 93.13 c $?.??

Safety Data: MSDS Toxic

Synonyms: benzamine; aminobenzene; aminophen; anilin; anilina; aniline oil; aniline reagent; anyvim; arylamine; benzene, amino-; benzidam; blue oil; C.I. 76000; C.I. oxidation base 1; cyanol; Huile D'aniline; krystallin; kyanol; NCI-C03736; phenylamine; Rcra waste number U012; UN 1547
Synthesis:    Prepare a mixture of 90 g of tin granules and 41.5 mL of nitrobenzene in a round bottom 1500-mL flask. Gradually add about 17 ml of concentrated hydrochloric acid, attach a reflux condenser, with or without water flowing, and shake the flask until thoroughly mixed. The flask will become warm after a short time, and a vigorous reaction can be observed. When this happens, immerse the flask in cold water to moderate the reaction. Add another 17 mL of hydrochloric acid and repeat the shaking/cooling process. Add a third and fourth portion of acid until approximately 80-85 mL of acid has been added, shaking and cooling each time. At this point the addition of acid should not give as quite a violent reaction, add an additional 85-90 mL of hydrochloric acid in larger portions. The total amount of acid added is 167 mL.
     After all of the acid has been added, the mixture is heated on a steam bath for 1 hour at reflux. After refluxing, add 100 mL of water to the flask. Prepare a solution of 150 g of sodium hydroxide in 200 mL of water, gradually add this solution to the flask in small portions. If the addition of the hydroxide solution causes the contents of the flask to boil, cool the flask in a water bath before adding more.
     To distill the aniline, set the flask up for steam distillation and distill, aniline and water will be collected. The initial distillate will be a milky color, when it becomes clear remove the collecting flask and add a new one. Collect an additional 300 mL of distillate.
     Combine the two distillate portions in an Erlenmeyer flask, and then add 25 g of finely powdered sodium chloride for every 100 mL of distillate collected. Shake the flask until all of the salt dissolves, then extract the solution with several portions of ether. Combine the ether portions, add a small amount of potassium hydroxide, and allow the ether to evaporate. The crude aniline thus obtained can be purified by simple distillation. The yield is 90-100%.

aniline hydrochloride C₆H₇N.HCl CAS number 142-04-1

mp 198 bp 245 d 1.2215 m 129.5889 c $?.??

Safety Data: MSDS

Synonyms: aniline chloride; aniline hydrochloride; aniline salt; anilinium chloride; benzenamine hydrochloride; C.I. 76001; hydrochloride benzenamine; phenylamine hydrochloride; phenylammonium chloride
Synthesis: Aniline hydrochloride is made by gradually adding concentrated hydrochloric acid to aniline. One method to test for completion is by placing a drop of solution on a piece of filter paper stained with methyl violet. If it turns green it is done. Otherwise add an excess of hydrochloric acid. After the acid has been added, cool the solution rapidly, with stirring, by placing it in a salt-ice bath. Small crystals of aniline hydrochloride will precipitate. Vacuum filter the solution to collect these crystals, press them with filter paper to squeeze out any excess water, and allow to dry.

aspirin C₉H₈O₄ CAS number 50-78-2

mp ? bp ? d ? m ? c $?.??

Safety Data: MSDS

Synonyms: 2-(acetyloxy)-benzoic acid ; ac 5230; acenterine; acesal; Acetaminophen Aspirin; acetate salicylic acid; aceticyl; acetilsalicilico; acetilum acidulatum; acetisal; acetonyl; acetophen; acetosal; acetosalic acid; acetosalin; 2-acetoxybenzoic acid; acetylin; acetylsal; acetylsalicylic acid; acetyl salycylic acid; acidum acetylsalicylicum; acimetten; acisal; acylpyrin; Alka-seltzer; Anacin; A.S.A.; a.s.a. empirin; asagran; asatard; Ascoden-30; Ascriptin; aspalon; aspergum; aspirdrops; Aspro; asteric; benaspir; bialpirinia; Bufferin; caprin; o-carboxyphenyl acetate; Chlorpheninaurine; colfarit; contrheuma retard; Coricidin; Coricidin D; cr; Darvon compound; duramax; ECM; Ecotrin; empirin; endydol; entericin; enterosarine; entrophen; Excedrin; extren; Gelprin; helicon; Measurin; Norgesic; Persistin; rhodine; Robaxisal; salacetin; salcetogen; saletin; salicylic acid acetate; Supac; Triaminicin; Vanquish; XAXA
Synthesis: Coming soon!

barium chloride BaCl₂ CAS number 10361-37-2

mp 963 bp - d 3.86 m 208.23 c $?.??

Safety Data: MSDS Toxic

Synonyms: ba 0108E; barium dichloride; NCI-C61074; SBA 0108E
Synthesis: Coming soon!

benzal chloride C₆H₅CHCl₂ CAS number 98-87-3

mp -17 bp 205 d 1.26 m 161.03 c $?.??

Safety Data: MSDS

Synonyms: benzylidene chloride; (dichloromethyl)benzene; benzyl dichloride; benzylene chloride; benzylidene dichloride; chlorobenzal; dichloro methyl-benzene; a,a-dichlorotoluene; dichlorophenylmethane
Synthesis:    Place 58 mL (50 g) of toluene in a round bottom 100-mL flask. Attach a Clasien adapter to the flask. On the angled arm of the adapter, attach a condenser set up for refluxing. Since excess chlorine gas will be released from the top of the condenser, affix a one-holed stopper with a short length of glass tubing connected to a long hose, direct the hose to a well ventilated area. On the straight arm of the adapter, attach a length of glass tubing with a bubbler at the end that extends below the surface of the toluene. The top of this tube is connected to a chlorine generator.
     Position the setup such that the flask is in direct sunlight, or very strong light. Sunlight is superior. Heat the toluene to boiling while a current of dry chlorine gas is bubbled in, the chlorine can be dried by passing it through two drying bottles filled with concentrated sulfuric acid. The course of the reaction is best judged by weighing the product; the reaction is complete when the toluene has increased by 40 g, the total weight being 90 g. By weighing the flask beforehand, and periodically interrupting the flow of chlorine to cool and weigh the flask, the completeness of the reaction can be determined. Without weighing, it is very difficult to gauge this reaction as the length varies greatly.
     In the summer, in direct midday sunlight, the reaction is complete in a few hours. In winter, or low light, the reaction needs 12-24 hours to complete. Adding 4 g of phosphorus pentachloride to the toluene can enhance the reaction. The crude benzal chloride thus obtained can be directly used to make benzaldehyde.

benzaldehyde C₇H₆O CAS number 100-52-7

mp -56.5 bp 179 d 1.043 m 106.12 c $?.??

Safety Data: MSDS

Synonyms: almond artificial essential oil; artificial almond oil; artificial bitter almond oil; artificial essential oil of almond; benzenecarbonal; benzene carboxaldehyde; benzene methylal; benzoic aldehyde; benzoyl hydride; oil of bitter almond; phenylmethanal
Synthesis:    To prepare benzaldehyde, start with the crude benzal chloride obtained from its synthesis. Into a round-bottomed flask with the benzal chloride, add a solution of 500 mL of water and 150 g of calcium carbonate. Set the flask up for reflux and heat for 4 hours on an oil bath. Keep the oil bath at 130 °C by checking the oil itself with a thermometer.
     After refluxing, steam distill the product to obtain crude benzaldehyde oil. (The portion that did not distill over contains some benzoic acid. It can be discarded, or purified by filtering while hot through a piece of fluted filter paper, then adding concentrated hydrochloric acid to the filtrate. On cooling the benzoic acid will precipitate, it is filtered and recrystallized from hot water.) The crude benzaldehyde oil is treated with a concentrated solution of sodium bisulfite, after shaking for a long time the oil should have dissolved into solution. If any crystals happen to form during the shaking, add water until they dissolve.
     After most of the oil is dissolved, filter the solution over fluted filter paper, and then treat the filtrate with sodium carbonate until it is strongly alkaline. This liquid is now steam distilled to obtain pure benzaldehyde. The product can be further purified by mixing with ether, letting the ether evaporate, and distilling (normal, not steam) the benzaldehyde.
     If you have obtained benzaldehyde from other sources, it must be purified if it is anything less than ACS grade. It should be washed with sodium carbonate solution, dried, and distilled with minimum atmospheric exposure. Only the fraction collected at 178-180 °C is kept.

benzaldehyde phenylhydrazone C₁₃H₁₂N₂ CAS number 588-64-7

mp 158 bp 327.5 d ? m 196.1 c $?.??

Safety Data: MSDS

Synonyms: benzalphenylhydrazine; benzylidenephenylhydrazine; diphenylhydrazone; NSC 37088
Synthesis: Prepare a solution of 9.81 g of benzaldehyde and 10 g of phenylhydrazine in 100 mL of ethyl alcohol. The benzaldehyde should be chilled to 0-5 degrees C before adding it to the solution. A cream colored solid should form; allow the solution to stand for 2 hours to complete the reaction. The solid is collected by vacuum filtration, washed with ice-cold ethyl alcohol, and dried under vacuum.

benzene C₆H₆ CAS number 71-43-2

mp 5.5 bp 80.1 d 0.8787 m 78.11 c $?.??

Safety Data: MSDS Flammable, Toxic

Synonyms: (6)annulene; benzine; benzol; benzolene; bicarburet of hydrogen; carbon oil; coal naphtha; cyclohexatriene; mineral naphtha; motor benzol; nitration benzene; phene; phenyl hydride; pyrobenzol
Synthesis: Nothing yet

bromine Br₂ CAS number 7726-95-6

mp ? bp ? d ? m ? c $?.??

Safety Data: MSDS

Synonyms:
Synthesis: Nothing yet

bromobenzene C₆H₅Br CAS number 108-86-1

mp -30.6 bp 156.2 d 1.4952 m 157.01 c $?.??

Safety Data: MSDS Flammable, Irritant

Synonyms: monobromobenzene; phenyl bromide
Synthesis:    To a 250-mL Florence flask connect a vertical tube 50 cm long and 1.5 cm wide, the upper end of which is closed by a stopper bearing a narrow glass tube bent at right angles to form a U. The other end is connected with a flask containing 250 mL of water, by a stopper having a small wedge removed. See the illustration. The tube does not touch the water, but remains about 1 cm above the surface. Place 57 mL of benzene and 1 g of iron filings into the first flask. Immerse the flask in a salt-ice bath to cool it down. Through the vertical tube add 40 mL of bromine, then immediately connect the narrow tube. After some time an extremely energetic reaction will begin with the evolution of hydrobromic acid gas, which should be completely absorbed by the water. Should there be no reaction after a short time, remove the ice bath for a brief period, and if necessary momentarily immerse the flask in warm water. As soon as even a weak gas evolution begins, the flask is at once cooled again. If you do not cool it right away there is a risk of the reaction going out of control, if this happens even with cooling, use larger iron filings or small nails.
     When the reaction has subsided remove the ice bath, dry the flask, and heat until no red bromine vapors are visible above the dark colored liquid. The product is shaken with several portions of water to wash it, and then steam distilled. As soon as crystals of dibromobenzene (some will always form) begin to separate out in the condenser, the receiver is changed and the distillation is continued until all of the dibromobenzene has passed over. The liquid portion is added to a seperatory funnel where the bromobenzene layer is collected, the water layer is discarded. Add the bromobenzene layer to a small Erlenmeyer flask, add a small amount of calcium chloride to dry it, shake the flask gently to mix it up. Filter the liquid to remove the calcium chloride, and then add it to a small round-bottomed Florence flask. Fractionally distill the liquid to collect pure bromobenzene. The portion distilling over between 140-170 °C is collected separately, this portion is fractionally distilled again, this time collecting only that which distills over at 150-160 °C. Yield is about 60-70 g.
     The residue boiling above 170 °C remaining the flask after the two distillations contains dibromobenzene and hydrobromic acid. These can be disposed of or, since bromine is quite valuable, purified and kept. Pour the residue, while still warm, onto a watch glass so it may cool. After cooling place the material, along with the other crystals of dibromobenzene, on a porous glass plate and press it to separate the acid. Add the pressed dibromobenzene to ethyl alcohol and recrystallize, it should now be quite pure. The hydrobromic acid that remains can be purified by fractional distillation. The fraction below 126 °C is water, which can be discarded. When the temperature reaches 126 and stays constant, begin collecting the distillate; this should be about 48% hydrobromic acid.

calcium carbonate CaCO₃ CAS number 471-34-1

mp 825 (dec) bp - d 2.83 m 100.09 c $?.??

Safety Data: MSDS

Synonyms: aglime; aragonite; atomite; Calcichew; Calcidia; Calcit; calcite; carbonic acid calcium salt (1:1); chalk; Citrical; limestone; marble; slaker rejects; vaterite; whiting
Synthesis: Coming soon!

calcium chloride CaCl₂ CAS number 10043-52-4

mp 772 bp 1600 d 2.152 m 110.98 c $?.??

Safety Data: MSDS Irritant

Synonyms: calcium dichloride; calcosan; intergravin-orales
Synthesis: Coming soon!

calcium hydroxide Ca(OH₂) CAS number 1305-62-0

mp - bp - d 2.08-2.34 m 74.09 c $?.??

Safety Data: MSDS Corrosive

Synonyms: calcium dihydroxide; calcium hydrate; carboxide; hydrated lime; lime, hydrated; lime water; slaked lime
Synthesis: Coming soon!

calcium hypophosphite Ca(H₂PO₂)₂ CAS number 7789-79-9

mp ? bp ? d ? m 170.05 c $?.??

Safety Data: MSDS

Synonyms:
Synthesis: Nothing yet

calcium sulfate CaSO₄ CAS number 7778-18-9

mp ? bp ? d ? m ? c $?.??

Safety Data: MSDS

Synonyms:
Synthesis: Nothing yet

carbanilide C₆H₅NHCONHC₆H₅ CAS number 102-07-8

mp 238 bp 260 (dec) d 1.239 m 212.25 c $?.??

Safety Data: MSDS

Synonyms: N,N'-diphenylurea; acardite; N,N'-difenylmocovina; diphenylcarbamide; diphenylurea; 1,3-diphenylurea; 3-diphenylurea; s-diphenylurea; sym-diphenylurea; karbanilid; N-phenyl-N'-phenylurea; urea, 1,3-diphenyl-; USAF ek-534
Synthesis:    Prepare a solution of 390 g of aniline hydrochloride and 190 g of urea in 1500 mL of water. Add the solution to a 3-L Florence flask and reflux at its boiling point for 2 hours. After reflux, rapidly suction filter the solution to collect the crystals, and then wash the carbanilide with 100 mL of boiling water. The filtrate is chilled, and the phenylurea that crystallizes out is filtered off and rinsed with a little cold water, the washing being discarded. The filtrate is again boiled under reflux for 2 hours, or until it begins to bump, and the filtration process is repeated. The filtrate is again refluxed and filtered a third time, and each time the phenylurea is collected from the cold filtrate. The filtrate is finally evaporated to half of its original volume, and additional crops of carbanilide and phenylurea are so obtained. The filtrate can now be discarded.
     The crude carbanilide can be purified be recrystallizing from ethyl alcohol with the use of some decolorizing carbon, you will need 1 L of alcohol per 25 g of carbanilide. The yield is about 40%. It may be more practical to use only a fraction of the reactants for this lab, say a tenth, and make multiple batches. The final purification can be done all at once.
     All of that phenylurea can be discarded, or kept, I know of no use for it. If you are keeping it, it can be purified by dissolving it in the minimum quantity of boiling water, adding a little decolorizing carbon, and filtering to remove any impurities. When the filtrate first begins to cool, a precipitate of carbanilide is deposited; this must be filtered off while the liquid is still hot. On cooling, pure phenylurea will precipitate. The yield here is about 50-55%.

carbon dioxide CO₂ CAS number 124-38-9

mp ? bp ? d ? m ? c $?.??

Safety Data: MSDS

Synonyms:
Synthesis: Nothing yet

carbon disulfide CS₂ CAS number 75-15-0

mp -111.6 bp 46.5 d 1.2632 m 76.14 c $?.??

Safety Data: MSDS Flammable, Toxic

Synonyms: alcohol of sulfur; carbon bisulfide; carbon bisulfuret; carbone; carbonio; carbon sulfide; dithiocarbonic anhydride; kohlendisulfid; koolstofdisulfide; NCI-C04591; Rcra waste number P022; schwefelkohlenstoff; solfuro di carbonio; sulfocarbonic anhydride; UN 1131; weeviltox; wegla dwusiarczek
Synthesis: Coming soon!

carbon tetrachloride CCl₄ CAS number 56-23-5

mp -23 bp 76.7 d 1.589 m 153.82 c $?.??

Safety Data: MSDS Toxic

Synonyms: tetrachloromethane; Benzinoform; carbona; carbon chloride; carbon tet; flukoids; methane tetrachloride; Necatorina; necatorine; perchloromethane; R 10 (refrigerant); refrigerant R10; tetrachlorocarbon; tetrafinol; tetraform; tetrasol; univerm; vermoestricid
Synthesis: Nothing yet

acetaldehyde			CH₃CHO	CAS number 75-07-0
mp -123.5	bp 21	d 0.788	m 44.05	c $?.??
Safety Data: MSDS Flammable			table key
Synonyms: acetic aldehyde; acetylaldehyde; aldehyde; ethanal; ethyl aldehyde; ethylaldehyde
Synthesis: Place 260 mL of 23% sulfuric acid in a 1500-mL Florence flask. Connect an addition funnel to the flask, and set it up for vacuum distillation with a 500-mL receiving flask. The receiving flask should be immersed in a salt-ice bath to cool the distillate when it comes over. Although a setup for vacuum distillation is used, it is not necessary to apply a vacuum; the vacuum adapter merely provides a means of equalizing pressure. Prepare a solution of 100 g of sodium dichromate in 200 mL of water and 127 mL of ethyl alcohol. Factor in the amount of water that is already in the ethyl alcohol when making the solution, i.e. 100 mL of 95% alcohol has 5 mL of water in it already. Place this solution in the addition funnel, position the stem of the funnel such that it is about 3 cm above the surface of the acid. Heat the acid until it just begins to boil, then add the mixture in the funnel in a steady stream to the acid. It will not be necessary to heat the flask during the addition because it will generate its own heat. The heat will be sufficient to distill over the acetaldehyde along with some alcohol and waste acetal. If acetaldehyde vapors begin to escape from the flask, regulate the distillation by decreasing the amount of dichromate solution being added. If the reaction flask does not boil on its own, gently heat it for a short time until boiling begins. The crude acetaldehyde thus obtained is difficult to distill from the alcohol and acetal mixed with it. It is therefore converted to aldehyde-ammonia, then back to pure aldehyde. Place the crude acetaldehyde in a Florence flask of suitable volume to contain no more than two thirds of the liquid. Attach a reflux condenser to the flask. Fill the condenser jacket with 30 °C water. It is only necessary to have the warm water in the jacket, not flowing. Stop up the lower connecter to prevent water from leaking out. To the top of the condenser, attach a glass tube connected to a wash bottle filled with 50 mL of ethyl ether. This wash bottle is then connected to another wash bottle filled with 50 mL of ether. After all connections have been made, the crude aldehyde is heated to a gentle boil for 5-10 minutes. The ether will absorb the acetaldehyde as it boils off. If the ether begins to rise up into the connecting tube from the condenser to the wash bottle, increase the heating. Combine the ether into a 150-mL beaker immersed in a salt-ice bath. Bubble dry ammonia gas into the ether through an inverted funnel or wide tube immersed near the bottom of the beaker. Add ammonia until the ethereal solution smells strongly of ammonia. After about an hour, pure ammonia-aldehyde should have separated out. Scrape the crystals from the beaker and collect them by suction filtration. Wash the crystals with a small amount of ether, and allow them to dry in a desiccator. The yield is about 30 g. To obtain pure acetaldehyde, dissolve 10 g of aldehyde-ammonia in 10 mL of water in a 50-mL Florence flask. Add 28 mL of cold 29% sulfuric acid to the flask and set it up for simple distillation. Heat the flask on a water bath to distill over the aldehyde. Place the receiving flask in a salt-ice bath to cool the volatile acetaldehyde. Acetaldehyde is extremely volatile and cannot be stored satisfactorily unless it is refrigerated or sealed in glass ampoules (not just capped), therefore it is necessary to prepare acetaldehyde each time it is needed. There is, however, an easier solution. A quick and easy way to store acetaldehyde is to polymerize it to paraldehyde, which can be handled and stored easily, then depolymerize when you need to use it. Now you can make a larger amount without worry. To polymerize acetaldehyde for storage, place it in a dry test tube and cautiously add 1 drop of concentrated sulfuric acid per 2 mL of acetaldehyde in the tube. Mix thoroughly, the polymerization will begin to take place. Some gentle warming can hasten the reaction. After some minutes add 3-4 mL of water per 2 mL of acetaldehyde, an insoluble precipitate of paraldehyde will form. As an aside, technically paraldehyde is a controlled substance. It is a sedative and a hypnotic drug useable by prescription only. To depolymerize paraldehyde back into acetaldehyde, place the paraldehyde into a round-bottom 200-mL Florence flask. Add 4-5 drops of concentrated sulfuric acid for every 20 g (20 mL) of paraldehyde in the flask. Set the flask up for fractional distillation, use glass in the fractionating column. Use a 125-mL Erlenmeyer flask as the receiver; keep it cool by immersing in an ice water (but not salt-ice) bath. Place a loose plug of cotton into the Erlenmeyer flask to help reduce evaporation loss; it must be loose. Care must be taken to prevent the cotton from coming into contact with the distillate. After setting up, heat the flask gently. The temperature of the distillate must not be allowed to rise above 35 °C as it will only repolymerize. The acetaldehyde is now ready for use.

acetamide			CH₃CONH₂	CAS number 60-35-5
mp 81	bp 222	d 1.159	m 59.07	c $?.??
Safety Data: MSDS
Synonyms: acetic acid amide; acetimidic acid; ethanamide; methanecarboxamide
Synthesis: Place 71.5 mL of glacial acetic acid into a ceramic or porcelain dish, heat the acid to 40-50 °C by a water bath. Neutralize the acid by adding 100 g of finely pulverized ammonium carbonate; the resulting compound should be slightly alkaline. The mass is warmed on the water bath to 80-90 °C until acidic, test for acidity by adding a few drops to a test tube of water then drop on litmus or pH paper. The reaction is now completed in a bomb tube, or Volhard tube, this is essentially a glass bottle that is sealed by melting the glass together at the opening. Since these may be hard to come by a substitute is needed. A heavy walled glass beer or wine bottle should lend itself well to acting as a reaction container. There is a strong possibility that such a bottle can burst under the great heat required of this reaction, this applies to the Volhard tube as well. The tube or bottle should be wrapped in a fine mesh metal screen, the kind used on windows, if it bursts the screen will prevent glass going everywhere. Heating the tube behind a sheet of wood is also a good idea. It will be quite necessary to melt the top of the glass closed; using a mere rubber or cork stopper is not sufficient because they will melt or burn. To seal the open end of a tube charged with the substance, it is warmed by holding it at an angle of about 45°, with constant turning, in the small luminous flame of a burner, and then heated strongly in the larger non-luminous flame. Heat the neck if using a bottle. When the glass becomes soft, use pliers to gently pull and squeeze the top of the tube upwards causing the glass of the neck to narrow. Continue to heat this narrowed portion and draw the top up until the glass has closed itself off. After breaking off or cutting of the end of the tip, to allow the air to escape on further heating, it is heated just below the top. When the tube is softened at this point it is drawn out slightly, heat is applied just below the top, it is drawn out again, and so on. The result is that the form of the top of the tube gradually changes from a cylinder to a sharp-pointed cone. The narrowest part of the cone is then heated without drawing it further. The soft glass melts together, and a thick walled cap is obtained. Fill the tube, previously heated by flame, with the compound while hot without using a funnel. If any portion adheres to the top of the tube, melt it down by carefully heating with a flame. Any remaining trace can be wiped away, now seal the tube as described above. Heat the tube for 5 hours at 220-230 °C in a furnace. After heating, break the bottle open to obtain the reaction product. The liquid product is fractionally distilled in a well ventilated area. The first fraction that distills over between 100-130 °C will be acetic acid and water. The temperature will then rise rapidly to 180 °C where upon acetamide will begin to distill over. Collect the portion distilling over between 180-230 °C in a beaker. Cool the beaker with a salt-ice bath towards the end of the distillation. Rub the walls of the beaker after the distillation to crystallize the impure acetamide. The crystals are placed on a Buchner funnel and pressed to squeeze out any liquids. The crystals are now simple distilled to obtain almost pure acetamide. To remove the last traces of impurities, again press the crystals, then recrystallize from a minimum amount of ethyl ether. Filter to collect the crystals, allow a brief period to dry. Yield is about 40 g.

acetic acid			CH₃COOH	CAS number 64-19-7
mp 16.7	bp 118	d 1.0492	m 60.05	c $?.??
Safety Data: MSDS Corrosive, Flammable
Synonyms: acetate; acetic acid glacial; Aci-Jel; ethanoic acid; ethylic acid; glacial acetic acid; methanecarboxylic acid; shotgun; TCLP extraction fluid 2; vinegar; vinegar acid
Synthesis: Acetic acid is available as an OTC chemical in the form of vinegar, a dilute solution of acetic acid. Vinegar should be available from any grocery story in 3%-5% concentrations or so. Acetic acid is a chemical that I consider to plentiful to bother synthesizing yourself since it is a cheap, abundant OTC chemical. It can be done, and it may be cheaper in the long run to make it on your own, but I do not have the information handy. A trip to the library, or a web search will yield much info on the topic. Acetic acid is more useful in concentrated, or glacial, form. Only acetic acid is referred to as glacial rather than concentrated acid. This is because the ancients liked how much frozen acetic acid looked, it reminded them of an ice glacier, so the term glacial stuck. Glacial acetic acid is very corrosive and slightly flammable. Vinegar can be made into glacial acetic acid by first converting it to sodium acetate. Once you have some sodium acetate ready, set up the necessary equipment for a simple distillation and fill the reaction flask with concentrated (95%+) sulfuric acid. Add the sodium acetate to the acid and begin the distillation. The sulfuric acid will break down the sodium acetate and the resulting acetic acid will distill off. The concentration of the acetic acid obtained will be nearly anhydrous, especially if you start with thoroughly dried sodium acetate and 100% sulfuric acid.

acetic anhydride			(CH₃CO)₂O	CAS number 108-24-7
mp -73	bp 139	d 1.080	m 102.09	c $?.??
Safety Data: MSDS Corrosive, Flammable
Synonyms: acetic acid anhydride; acetic oxide; acetyl anhydride; acetyl ether; acetyl oxide; ethanoic anhydrate; ethanoic anhydride
Synthesis: Acetic anhydride is a very handy organic compound that has fallen into ill repute thanks to the drug dealers. It is technically a watched chemical, but you will only have to answer questions at gunpoint if you buy over 250 gallons. Even so, you will most likely be put on The List if you buy any, and you will have to come up with a bunch of explanations as to what you are going to do with it. Acetic anhydride is very corrosive and must be kept away from moisture, as it will decompose into acetic acid. Into a 200-mL Florence flask, add 70 g of finely pulverized, anhydrous sodium acetate. Set the flask up for simple distillation, instead of a thermometer in the top of the flask use an addition funnel. Slowly add, by dropwise addition, 45.5 mL of acetyl chloride from the addition funnel. After half of the acetyl chloride has been added, stop the addition and stir the reaction mix with a glass stirring rod. Afterwards, continue the addition the rest of the way. If at any point during the addition some material should distill over, pour it back into the reaction flask and decrease the rate of addition to prevent this. After the addition is complete, remove the addition funnel, stop up the flask, and distill with flame or hot plate. The crude acetic anhydride thus obtained needs to be purified by distillation. Set up for a simple distillation, add 3 g of finely pulverized, anhydrous sodium acetate to the reaction flask, and then pour in the crude acetic anhydride. The sodium acetate will convert any remaining acetyl chloride into the anhydride. The receiving flask should be under a water shower for cooling. Place a large funnel (a cheap plastic one will work fine) under the flask with a tube leading to the sink, pour cold water over the top of the receiving flask. The receiving flask can also be held directly under the faucet in the sink. Commence the distillation; the yield should be about 50 g of pure acetic anhydride.

acetone			CH₃COCH₃	CAS number 67-64-1
mp -94	bp 56.5	d 0.788	m 58.08	c $?.??
Safety Data: MSDS Flammable
Synonyms: 2-propanone; chevron acetone; dimethyl formaldehyde; dimethylketal; dimethyl ketone; ketone propane; beta-ketopropane; methyl ketone; propanone; pyroacetic acid; pyroacetic ether
Synthesis: Acetone is available as an OTC chemical in just about every hardware store. The stores sell it cheap, pure, and in large quantities. As far as Synthesis goes it is rather complicated, so it is best to purchase it. Its primary use in the household is as a solvent for paint, i.e. thinning paint, removing varnishes, and cleaning brushes. It can be purchased in pint to 5-gallon sizes at hardware stores or paint supply stores without question. Acetone can be dried out by adding a small amount of calcium chloride, say 1 g per 25 mL, and letting it stand for three to seven days in a sealed container. Occasional agitation, every 12-24 hours, will improve the drying process. After letting the acetone stand, distill it to get the dry acetone. Some of the acetone will combine with the calcium chloride, so it necessary to distill it. Store the dry acetone in a well-sealed container.

acetyl chloride			CH₃COCl	CAS number 75-36-5
mp -112	bp 52	d 1.104	m 78.50	c $?.??
Safety Data: MSDS
Synonyms: acetic acid chloride; acetic chloride; ethanoyl chloride
Synthesis: Place 95 mL of glacial acetic acid into a round-bottomed 500-mL Florence flask. Set the flask up for vacuum distillation with addition. Instead of connecting the vacuum adapter to a vacuum source, attach a calcium chloride drying tube. There is no need for vacuum, just an airtight connection to protect the product from moisture. While cooling the flask in a salt-ice bath, slowly add 51 mL of phosphorus trichloride through the addition funnel. After the addition, place the flask in a water bath heated to 40-50 °C. Continue heating until the active evolution of hydrochloric acid gas slackens, and the liquid separates into two layers. To separate the acetyl chloride, which should have formed on the upper layer, heat the flask on a boiling water bath until nothing more distills over. To purify the acetyl chloride, simple distill the product obtained in the same apparatus used before, except this time replace the addition funnel with a thermometer. Collect the portion distilling over from 50 to 56 °C. The yield is about 80-90 g.

acrylic acid			CH₂=CHCO₂H	CAS number 79-10-7
mp 14	bp 141.0	d 1.0621	m 72.06	c $?.??
Safety Data: MSDS Corrosive, Flammable
Synonyms: 2-propenoic acid; acroleic acid; acrylate; ethylenecarboxylic acid; propene acid; propenoic acid; vinylformic acid
Synthesis: Prepare a mixture of 151 mL of 98-100% formic acid, 1060 mL of methyl acrylate, 30 g of hydroquinone, and 2 mL of sulfuric acid in a round-bottomed 2-L flask. Set the flask up for refluxing. Reflux with an oil bath heated to 85-95 °C (the oil not the contents of the flask) for 1-3 hours. Remove the reflux column and set the flask up for fractional distillation, using copper sponge to pack the column. Slowly distill the mixture at 32-35 °C for about 8-10 hours, you will be removing methyl formate waste from the mixture. You will want to let 1 drop of distillate come over for every 5 that fall back into the flask, then allow more to come over near the end. When no more methyl formate is produced, the excess methyl acrylate is fractionally distilled under partial vacuum at 32-35 °C with the oil temperature at 60-65 °:C. Reconfigure the setup for vacuum distillation if need be. You will also need to add a clasien adapter so as to extend a length of tubing into the mixture. During the distillation, a slow stream of carbon dioxide is admitted through this tube. When all the methyl acrylate has been removed, the acrylic acid is fractionally distilled at 53-56 °C under vacuum. Upon redistillation acrylic acid of 97% purity is obtained in a yield of 74-78% or about 220-230 g.

acrylyl chloride			H₂C=CHCOCl	CAS number 814-68-6
mp ?	bp 72-76	d 1.1140	m 90.51	c $?.??
Safety Data: MSDS Corrosive, Flammable
Synonyms: acryl chloride; acrylic acid chloride; acryloyl chloride; chlorid kyseliny akrylove; 2-propenoyl chloride; propenoyl chloride
Synthesis: Into a 1-L round-bottomed flask place 135 mL of thionyl chloride. Set this flask up for refluxing with addition. Heat the thionyl chloride to boiling, and then add 115 mL of acrylic acid at such a rate that the mixture refluxes gently. It may require about an hour to add all of the acid. This reaction will generate toxic sulfur dioxide gas, so take the necessary precautions. After all of the acid has been added, continue to reflux for an additional 30 minutes to expel all of the sulfur dioxide gas. I have no information on how to isolate or purify this chemical. It will be mixed with hydrochloric acid as a waste byproduct. I would suggest neutralizing the acid by adding some sodium hydroxide, and then distilling the product to get pure acrylyl chloride. If using this chemical to make 1,1,1-trinitro-2-propyl acrylate, try using aluminum hydroxide to neutralize the acid. The product of this is aluminum chloride, which is needed in the reaction, so no need to distill this.

allyl methanesulfonate			C₄H₈O₃S	CAS number 6728-21-8
mp ?	bp ?	d ?	m 136.1	c $?.??
Safety Data: MSDS
Synonyms: allyl mesylate; methanesulfonic acid, allyl ester; methanesulfonic acid, 2-propenyl ester
Synthesis: In a 1000-mL Erlenmeyer flask prepare a solution of 20 g of distilled allyl alcohol (98%) in 300 mL of diethyl ether. Cool the flask in an ice-water bath to below 5 degrees C. With stirring add 56.5 g of solid potassium carbonate in one portion; next add 3.3 g of solid trimethylamine hydrochloride in one portion. Stir the resulting suspension for 5 minutes. With vigorous stirring add 46.9 g of methanesulfonyl chloride to the flask dropwise over a period of 1 hour. After the addition of methanesulfonyl chloride is complete continue stirring the contents of the flask for 5 hours and maintain the temperature at 5 degrees C. Next add 300 mL of water to the flask and continue to stir the contents vigorously for an additional 15 minutes before discontinuing the stirring. Allow the contents of the flask to separate into two layers, the aqueous layer will be on the bottom. Decant off as much of the aqueous layer as possible by a pipette and collect it in a separate beaker. Mix the aqueous portion with two portions of 100 mL of ethyl ether and shake them in a seperatory funnel. It may be necessary to break up the aqueous layer into four batches to fit into the seperatory funnel, in which case shake each 75 mL portion of water with two 25 mL portions of ether. Combine all of the ether extracts with the organic layer in an Erlenmeyer flask and add a portion of anhydrous magnesium sulfate to draw out any moisture. Remove the ether by evaporating under reduced pressure without heating. The remaining allyl methanesulfonate is poured over a filter to remove the magnesium sulfate and kept under high vacuum to remove any final traces of solvent. What remains should be about 38-39 g of clear colorless oil. Yield is 83%. If possible this reaction should be carried out under an atmosphere of nitrogen.

aluminum			Al	CAS number 7429-90-5
mp 660	bp 2327	d 2.70	m 26.981539	c $?.??
Safety Data: MSDS Flammable
Synonyms: aluminium
Synthesis: Aluminum powder will add explosive strength to just about any high explosive. The powder only that is, not foil or wire. The kind of powder needed is very finely divided, not the kind that can be purchased from automotive stores as a leak plugger for the radiator, that variety is too coarse. The only possible OTC source is from paint stores as an additive for paint. I should mention that I have never seen it sold in paint stores. If all else fails one can buy finely powered aluminum from chemical suppliers who deal with the public. Companies that sell pyrotechnic materials will in all likelihood have several grades available from coarse down to atomized. When using aluminum in chemical reactions one can use aluminum foil available at any grocery store, or aluminum tubing or rod available at hardware stores. Aluminum products are quite abundant at many stores. Aluminum foil is quite versatile because it offers a higher surface area compared to other types of OTC aluminum, it is quite cheap, and is pure. Aluminum foil is easy to tear into a desired mass and can be crumpled into balls of any size if coarse bits are needed for a reaction. Aluminum tubing or rod will need to be machined to get turnings, chunks, or shot which sounds like a lot work and special equipment.

aluminum chloride			AlCl₃	CAS number 7446-70-0
mp ?	bp ?	d ?	m 133.34	c $?.??
Safety Data: MSDS Corrosive
Synonyms: AlCl3; alluminio(cloruro di); aluminiumchlorid; aluminium, (chlorure d'); aluminium trichloride; aluminum chloride (1:3); chlorure d'aluminium; Drysol; NSC 143016; PAC (salt); Pearsall; trichloroaluminum; UN 1726; UN 2581
Synthesis: The Synthesis of aluminum chloride will require a creative glassware setup. Assemble a heating apparatus as shown in the illustration below; each part must be completely dry for the reaction to work. The long furnace tube of hard glass should be 1.5 to 2 cm in diameter. The length is up to you, but a tube of 25-40 cm should suffice. One end of the tube can be drawn out to a narrow aperture if desired, since that requires some glassblowing skill it may be difficult for the improviser. A stopper with a short length of glass tubing in the middle will do nicely. The wide end of the tube is inserted into the center of a large stopper, a second glass tube, of at least 8 mm diameter, bent at a right angle, is placed above the larger. The large stopper is then attached to a wide mouth glass bottle. The part of the tube extending beyond the flames must be as short as possible to prevent the product from condensing prematurely, or it will clog the tube. Each end of the tube is plugged with glass wool to keep the reactants inside. A heat resistant plate is secured between the bottle and the flame to protect the stopper from burning or melting, you can use glass wool, aluminum foil, or any kind of fire resistant material (asbestos was recommended, it is now unavailable). If you have a stopper at the other end instead of a narrowed end, you will need a plate there too. Fill the glass tube half way (horizontally, not vertically) with aluminum shavings before assembling of course. You can use little aluminum foil balls, or machine shop shavings, the latter must be cleaned of oil by boiling in ethyl alcohol and dried in an oven at 120 °C. A very rapid current of dry hydrogen chloride gas is passed into the tube from the narrow end; the gas first passes into two drying bottles filled with concentrated sulfuric acid. Do not fill the bottles with too much acid as it can foam up. Test to see if all of the air has been removed from the apparatus by connecting a rubber hose to the angled outlet tube and directing the gas into a beaker of water. When only HCl gas remains, it will be absorbed directly into the water with little or no bubbling, now remove the tubing. If any air remains, there can be an explosion of oxygen and hydrogen. Now that the air is out, begin heating the tube with several burners along its length. Start with small flames and gradually increase. White vapors of aluminum chloride will begin to be evolved when the flames are high enough, and will be condensed into the bottle. Do not heat the aluminum so high it melts, if this happens remove the flames immediately. Continue heating when it solidifies. The reaction is done when all of the aluminum has been consumed, a small amount of dark residue may remain. The current of hydrogen chloride gas must be kept constantly rapid for this reaction to work. The aluminum chloride thus obtained is quite pure; store it in tightly sealed bottles or a desiccator.

aminoguanidine bicarbonate			C₂H₈N₄O₃	CAS number 2582-30-1
mp ?	bp ?	d ?	m ?	c $?.??
Safety Data: MSDS Irritant
Synonyms: aminoguanidinium hydrogen carbonate; carbonic acid with hydrazinecarboximidamide (1:1)
Synthesis: Two hundred and sixteen grams (2.07 moles) of nitroguanidine1 and 740 g. (11.3 moles) of purified zinc dust (Note 1) are thoroughly ground together in a mortar, and then enough water (about 400 ml.) is added with stirring with the pestle to form a thick paste. The paste is transferred to a 3-l. enameled can or beaker surrounded by an ice bath. A solution of 128 g. (2.14 moles) of glacial acetic acid in 130 ml. of water is cooled to 5� in another 3-l. beaker, which is fitted with a strong mechanical stirrer and surrounded by an ice bath. The paste of nitroguanidine and zinc dust, cooled to 5�, is added slowly with mechanical stirring, the temperature of the reaction mixture being kept between 5� and 15�. A total of about 1 kg. of cracked ice is added to the mixture from time to time as the mixture becomes too warm or too thick to stir. The addition of the paste takes about 8 hours, and the final volume of the mixture is about 1.5 l. (Note 2). The mixture is then slowly warmed to 40� on a water bath with continued stirring, and this temperature is maintained for 1�5 minutes, until reduction is complete (Note 3). The solution is immediately separated from the insoluble material by filtration on a 20-cm. B�chner funnel, and the cake is sucked as dry as possible. The residue is transferred to the 3-l. beaker, triturated well with 1 l. of water, and then separated from the liquid by filtration. In the same manner, the residue is washed twice more with two 600-ml. portions of water. The filtrates are combined and placed in a 5-l. round-bottomed flask. Two hundred grams of ammonium chloride is added, and the solution is mechanically stirred until solution is complete (Note 4). The stirring is continued, and 220 g. (2.62 moles) of sodium bicarbonate is added during a period of about 10 minutes. The aminoguanidine bicarbonate begins to precipitate after a few minutes, and the solution is then placed in a refrigerator overnight. The precipitate is collected by filtration on a B�chner funnel. The cake is removed to a 1-l. beaker and mixed with a 400-ml. portion of a 5% solution of ammonium chloride and filtered. It is again washed with two 400-ml. portions of distilled water, the wash solution being removed each time by filtration. Finally the solid is pressed down on the B�chner funnel; the mat is broken up with a spatula and washed while on the funnel with two 400-ml. portions of 95% ethanol and then with one 400-ml. portion of ether. After air drying, the aminoguanidine bicarbonate amounts to 180�182 g. (63�64%) of a white solid, melting at 172� with decomposition (Note 5) and (Note 6). 1. The zinc is purified by stirring 1.2 kg. of commercial zinc dust with 3 l. of 2% hydrochloric acid for 1 minute. The acid is removed by filtration, and the zinc is washed in a 4-l. beaker with one 3-l. portion of 2% hydrochloric acid, three 3-l. portions of distilled water, two 2-l. portions of 95% ethanol, and finally with one 2-l. portion of absolute ether, the wash solutions being removed each time by filtration. Then the material is thoroughly dried and any lumps are broken up in a mortar. 2. The solution becomes basic to litmus after one-half to three-fourths of the paste has been added. Lower yields are obtained if a larger excess of acetic acid is employed. 3. The state of reduction can be determined by placing 3 drops of the reaction mixture in a test tube containing 5 ml. of a 10% solution of sodium hydroxide and then adding 5 ml. of a freshly prepared saturated solution of ferrous ammonium sulfate. A red coloration indicates incomplete reduction; when the reduction is complete, only a greenish precipitate is observed. The mixture should not be heated after this test shows that reduction is complete. 4. The presence of the ammonium chloride prevents the coprecipitation of zinc salts when sodium bicarbonate is added to the solution to precipitate the aminoguanidine as the bicarbonate. If the solution is not clear at this step, it should be filtered. 5. The aminoguanidine bicarbonate is pure enough for most purposes. It should not be recrystallized from hot water, since decomposition will occur. 6. W. W. Hartman and Ross Philips have submitted a procedure suitable for the preparation of aminoguanidine bicarbonate on a larger scale. The sulfates of methylisothiourea and of hydrazine are allowed to react with the evolution of methyl mercaptan. In a 30-gal. crock are placed 10 l. of water and 5760 g. (20 moles) of methylisothiourea sulfate.2 In a 22-l. flask, 5.2 kg. (40 moles) of hydrazine sulfate3 is stirred with 12 l. of water, and 40% sodium hydroxide is added until all the hydrazine sulfate has dissolved and the solution is just neutral to Congo paper. The exact amount of alkali is noted and a duplicate amount added. The hydrazine solution is then added to the 30-gal. crock with stirring, as fast as possible, without allowing the foam to overflow the crock. The mixing is done out-of-doors, or in an efficient hood, since large volumes of methyl mercaptan are evolved. If the reaction is carried out on a smaller scale in 12- or 22-l. flasks, using appropriate amounts of material, the methyl mercaptan evolved may be absorbed in cold sodium hydroxide solution and isolated if desired. The solution is stirred until evolution of mercaptan stops, and then a few liters of water are distilled off under reduced pressure to free the solution entirely from mercaptan. The residual liquor is chilled in a crock, and a crop of hydrated sodium sulfate is filtered off, washed with ice water, and discarded. The filtrate is warmed to 20�25�, 25 ml. of glacial acetic acid is added, then 4 kg. of sodium bicarbonate, and the solution is stirred vigorously for 5 minutes and thereafter occasionally during an hour, or until the precipitate no longer increases. The precipitate is filtered with suction and washed with ice water and then with methanol, and is dried at a temperature not above 60�70�. The yield is 3760 g. (69% of the theoretical amount). Hydrazine sulfate may be recovered from the final filtrate, if the filtrate is strongly acidified with sulfuric acid and allowed to cool. This procedure borrowed from Organic Synthesis Collective Volume 3 pg 73

ammonia			NH₃	CAS number 7664-41-7
mp -77.7	bp -33.35	d 0.6818	m 17.03	c $?.??
Safety Data: MSDS Corrosive, Irritant, Toxic
Synonyms: N-H
Synthesis: One method gaseous ammonia can be generated is by heating a small flask full of the most concentrated ammonium hydroxide available with a burner, household hydroxide will not be sufficient. The gas can be dried by passing it through a drying tube filled with a mixture of 4 parts calcium oxide with 1 part sodium hydroxide.

ammonium carbonate			(NH₄)₂CO₃	CAS number 506-87-6
mp ?	bp ?	d ?	m ?	c $?.??
Safety Data: MSDS
Synonyms: ammonium sesquicarbonate; carbonic acid, ammonium salt; carbonic acid, diammonium salt; crystal ammonia; diammonium carbonate; hartshorn
Synthesis: Coming soon!

ammonium chloride			NH₄Cl	CAS number 12125-02-9
mp ?	bp ?	d 1.5274	m 53.49	c $?.??
Safety Data: MSDS
Synonyms: Amchlor; ammoneric; ammoniumchlorid; ammonium muriate; chlorid amonny; Darammon; sal ammonia; sal ammoniac; salammonite; salmiac
Synthesis: Coming soon!

ammonium ferrous sulfate			(NH₄)₂Fe(SO₄)₂ � 6 H₂O	CAS number 10045-89-3
mp 100 (dec)	bp -	d 1.86	m 284.05	c $?.??
Safety Data: MSDS
Synonyms: ammonium iron sulfate; ferrous ammonium sulfate; iron ammonium sulfate; Mohr's salt; sulfuric acid, ammonium iron(2+) salt
Synthesis: Prepare a solution of 234 g of ammonium bisulfate in 1 L of water. Add 42.7 g iron metal to the solution and heat to 70 degrees C until all of the iron dissolves (reacts). Add an additional 234 g of ammonium bisulfate to the solution and again add 42.7 g of iron and heat to 70 degrees until all of the iron reacts. Cool the solution down to less than 15 degrees C with stirring; ammonium ferrous sulfate should then precipitate. Pour the liquid over a filter to collect the crystals. You may need to boil the liquid down to half its volume to obtain a complete crop of crystals. The ammonium bisulfate used in this reaction can be obtained by heating ammonium sulfate to 370 degrees C and cooking for about 15-20 minutes. Ammonium sulfate can be obtained either as fertilizer or by reacting ammonia with sulfuric acid.

ammonium hydroxide			NH₄OH	CAS number 1336-21-6
mp -	bp -	d 0.90	m -	c $?.??
Safety Data: MSDS Corrosive
Synonyms: ammonia, monohydrate; ammonia water; ammonium, aqueous; aqua ammonia; aqueous ammonia; Spirit of Hartshorn
Synthesis: Coming soon!

aniline			C₆H₅NH₂	CAS number 62-53-3
mp -6	bp 184-186	d 1.022	m 93.13	c $?.??
Safety Data: MSDS Toxic
Synonyms: benzamine; aminobenzene; aminophen; anilin; anilina; aniline oil; aniline reagent; anyvim; arylamine; benzene, amino-; benzidam; blue oil; C.I. 76000; C.I. oxidation base 1; cyanol; Huile D'aniline; krystallin; kyanol; NCI-C03736; phenylamine; Rcra waste number U012; UN 1547
Synthesis: Prepare a mixture of 90 g of tin granules and 41.5 mL of nitrobenzene in a round bottom 1500-mL flask. Gradually add about 17 ml of concentrated hydrochloric acid, attach a reflux condenser, with or without water flowing, and shake the flask until thoroughly mixed. The flask will become warm after a short time, and a vigorous reaction can be observed. When this happens, immerse the flask in cold water to moderate the reaction. Add another 17 mL of hydrochloric acid and repeat the shaking/cooling process. Add a third and fourth portion of acid until approximately 80-85 mL of acid has been added, shaking and cooling each time. At this point the addition of acid should not give as quite a violent reaction, add an additional 85-90 mL of hydrochloric acid in larger portions. The total amount of acid added is 167 mL. After all of the acid has been added, the mixture is heated on a steam bath for 1 hour at reflux. After refluxing, add 100 mL of water to the flask. Prepare a solution of 150 g of sodium hydroxide in 200 mL of water, gradually add this solution to the flask in small portions. If the addition of the hydroxide solution causes the contents of the flask to boil, cool the flask in a water bath before adding more. To distill the aniline, set the flask up for steam distillation and distill, aniline and water will be collected. The initial distillate will be a milky color, when it becomes clear remove the collecting flask and add a new one. Collect an additional 300 mL of distillate. Combine the two distillate portions in an Erlenmeyer flask, and then add 25 g of finely powdered sodium chloride for every 100 mL of distillate collected. Shake the flask until all of the salt dissolves, then extract the solution with several portions of ether. Combine the ether portions, add a small amount of potassium hydroxide, and allow the ether to evaporate. The crude aniline thus obtained can be purified by simple distillation. The yield is 90-100%.

aniline hydrochloride			C₆H₇N.HCl	CAS number 142-04-1
mp 198	bp 245	d 1.2215	m 129.5889	c $?.??
Safety Data: MSDS
Synonyms: aniline chloride; aniline hydrochloride; aniline salt; anilinium chloride; benzenamine hydrochloride; C.I. 76001; hydrochloride benzenamine; phenylamine hydrochloride; phenylammonium chloride
Synthesis: Aniline hydrochloride is made by gradually adding concentrated hydrochloric acid to aniline. One method to test for completion is by placing a drop of solution on a piece of filter paper stained with methyl violet. If it turns green it is done. Otherwise add an excess of hydrochloric acid. After the acid has been added, cool the solution rapidly, with stirring, by placing it in a salt-ice bath. Small crystals of aniline hydrochloride will precipitate. Vacuum filter the solution to collect these crystals, press them with filter paper to squeeze out any excess water, and allow to dry.

aspirin			C₉H₈O₄	CAS number 50-78-2
mp ?	bp ?	d ?	m ?	c $?.??
Safety Data: MSDS
Synonyms: 2-(acetyloxy)-benzoic acid ; ac 5230; acenterine; acesal; Acetaminophen Aspirin; acetate salicylic acid; aceticyl; acetilsalicilico; acetilum acidulatum; acetisal; acetonyl; acetophen; acetosal; acetosalic acid; acetosalin; 2-acetoxybenzoic acid; acetylin; acetylsal; acetylsalicylic acid; acetyl salycylic acid; acidum acetylsalicylicum; acimetten; acisal; acylpyrin; Alka-seltzer; Anacin; A.S.A.; a.s.a. empirin; asagran; asatard; Ascoden-30; Ascriptin; aspalon; aspergum; aspirdrops; Aspro; asteric; benaspir; bialpirinia; Bufferin; caprin; o-carboxyphenyl acetate; Chlorpheninaurine; colfarit; contrheuma retard; Coricidin; Coricidin D; cr; Darvon compound; duramax; ECM; Ecotrin; empirin; endydol; entericin; enterosarine; entrophen; Excedrin; extren; Gelprin; helicon; Measurin; Norgesic; Persistin; rhodine; Robaxisal; salacetin; salcetogen; saletin; salicylic acid acetate; Supac; Triaminicin; Vanquish; XAXA
Synthesis: Coming soon!

barium chloride			BaCl₂	CAS number 10361-37-2
mp 963	bp -	d 3.86	m 208.23	c $?.??
Safety Data: MSDS Toxic
Synonyms: ba 0108E; barium dichloride; NCI-C61074; SBA 0108E
Synthesis: Coming soon!

benzal chloride			C₆H₅CHCl₂	CAS number 98-87-3
mp -17	bp 205	d 1.26	m 161.03	c $?.??
Safety Data: MSDS
Synonyms: benzylidene chloride; (dichloromethyl)benzene; benzyl dichloride; benzylene chloride; benzylidene dichloride; chlorobenzal; dichloro methyl-benzene; a,a-dichlorotoluene; dichlorophenylmethane
Synthesis: Place 58 mL (50 g) of toluene in a round bottom 100-mL flask. Attach a Clasien adapter to the flask. On the angled arm of the adapter, attach a condenser set up for refluxing. Since excess chlorine gas will be released from the top of the condenser, affix a one-holed stopper with a short length of glass tubing connected to a long hose, direct the hose to a well ventilated area. On the straight arm of the adapter, attach a length of glass tubing with a bubbler at the end that extends below the surface of the toluene. The top of this tube is connected to a chlorine generator. Position the setup such that the flask is in direct sunlight, or very strong light. Sunlight is superior. Heat the toluene to boiling while a current of dry chlorine gas is bubbled in, the chlorine can be dried by passing it through two drying bottles filled with concentrated sulfuric acid. The course of the reaction is best judged by weighing the product; the reaction is complete when the toluene has increased by 40 g, the total weight being 90 g. By weighing the flask beforehand, and periodically interrupting the flow of chlorine to cool and weigh the flask, the completeness of the reaction can be determined. Without weighing, it is very difficult to gauge this reaction as the length varies greatly. In the summer, in direct midday sunlight, the reaction is complete in a few hours. In winter, or low light, the reaction needs 12-24 hours to complete. Adding 4 g of phosphorus pentachloride to the toluene can enhance the reaction. The crude benzal chloride thus obtained can be directly used to make benzaldehyde.

benzaldehyde			C₇H₆O	CAS number 100-52-7
mp -56.5	bp 179	d 1.043	m 106.12	c $?.??
Safety Data: MSDS
Synonyms: almond artificial essential oil; artificial almond oil; artificial bitter almond oil; artificial essential oil of almond; benzenecarbonal; benzene carboxaldehyde; benzene methylal; benzoic aldehyde; benzoyl hydride; oil of bitter almond; phenylmethanal
Synthesis: To prepare benzaldehyde, start with the crude benzal chloride obtained from its synthesis. Into a round-bottomed flask with the benzal chloride, add a solution of 500 mL of water and 150 g of calcium carbonate. Set the flask up for reflux and heat for 4 hours on an oil bath. Keep the oil bath at 130 °C by checking the oil itself with a thermometer. After refluxing, steam distill the product to obtain crude benzaldehyde oil. (The portion that did not distill over contains some benzoic acid. It can be discarded, or purified by filtering while hot through a piece of fluted filter paper, then adding concentrated hydrochloric acid to the filtrate. On cooling the benzoic acid will precipitate, it is filtered and recrystallized from hot water.) The crude benzaldehyde oil is treated with a concentrated solution of sodium bisulfite, after shaking for a long time the oil should have dissolved into solution. If any crystals happen to form during the shaking, add water until they dissolve. After most of the oil is dissolved, filter the solution over fluted filter paper, and then treat the filtrate with sodium carbonate until it is strongly alkaline. This liquid is now steam distilled to obtain pure benzaldehyde. The product can be further purified by mixing with ether, letting the ether evaporate, and distilling (normal, not steam) the benzaldehyde. If you have obtained benzaldehyde from other sources, it must be purified if it is anything less than ACS grade. It should be washed with sodium carbonate solution, dried, and distilled with minimum atmospheric exposure. Only the fraction collected at 178-180 °C is kept.

benzaldehyde phenylhydrazone			C₁₃H₁₂N₂	CAS number 588-64-7
mp 158	bp 327.5	d ?	m 196.1	c $?.??
Safety Data: MSDS
Synonyms: benzalphenylhydrazine; benzylidenephenylhydrazine; diphenylhydrazone; NSC 37088
Synthesis: Prepare a solution of 9.81 g of benzaldehyde and 10 g of phenylhydrazine in 100 mL of ethyl alcohol. The benzaldehyde should be chilled to 0-5 degrees C before adding it to the solution. A cream colored solid should form; allow the solution to stand for 2 hours to complete the reaction. The solid is collected by vacuum filtration, washed with ice-cold ethyl alcohol, and dried under vacuum.

benzene			C₆H₆	CAS number 71-43-2
mp 5.5	bp 80.1	d 0.8787	m 78.11	c $?.??
Safety Data: MSDS Flammable, Toxic
Synonyms: (6)annulene; benzine; benzol; benzolene; bicarburet of hydrogen; carbon oil; coal naphtha; cyclohexatriene; mineral naphtha; motor benzol; nitration benzene; phene; phenyl hydride; pyrobenzol
Synthesis: Nothing yet

bromine			Br₂	CAS number 7726-95-6
mp ?	bp ?	d ?	m ?	c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

bromobenzene			C₆H₅Br	CAS number 108-86-1
mp -30.6	bp 156.2	d 1.4952	m 157.01	c $?.??
Safety Data: MSDS Flammable, Irritant
Synonyms: monobromobenzene; phenyl bromide
Synthesis: To a 250-mL Florence flask connect a vertical tube 50 cm long and 1.5 cm wide, the upper end of which is closed by a stopper bearing a narrow glass tube bent at right angles to form a U. The other end is connected with a flask containing 250 mL of water, by a stopper having a small wedge removed. See the illustration. The tube does not touch the water, but remains about 1 cm above the surface. Place 57 mL of benzene and 1 g of iron filings into the first flask. Immerse the flask in a salt-ice bath to cool it down. Through the vertical tube add 40 mL of bromine, then immediately connect the narrow tube. After some time an extremely energetic reaction will begin with the evolution of hydrobromic acid gas, which should be completely absorbed by the water. Should there be no reaction after a short time, remove the ice bath for a brief period, and if necessary momentarily immerse the flask in warm water. As soon as even a weak gas evolution begins, the flask is at once cooled again. If you do not cool it right away there is a risk of the reaction going out of control, if this happens even with cooling, use larger iron filings or small nails. When the reaction has subsided remove the ice bath, dry the flask, and heat until no red bromine vapors are visible above the dark colored liquid. The product is shaken with several portions of water to wash it, and then steam distilled. As soon as crystals of dibromobenzene (some will always form) begin to separate out in the condenser, the receiver is changed and the distillation is continued until all of the dibromobenzene has passed over. The liquid portion is added to a seperatory funnel where the bromobenzene layer is collected, the water layer is discarded. Add the bromobenzene layer to a small Erlenmeyer flask, add a small amount of calcium chloride to dry it, shake the flask gently to mix it up. Filter the liquid to remove the calcium chloride, and then add it to a small round-bottomed Florence flask. Fractionally distill the liquid to collect pure bromobenzene. The portion distilling over between 140-170 °C is collected separately, this portion is fractionally distilled again, this time collecting only that which distills over at 150-160 °C. Yield is about 60-70 g. The residue boiling above 170 °C remaining the flask after the two distillations contains dibromobenzene and hydrobromic acid. These can be disposed of or, since bromine is quite valuable, purified and kept. Pour the residue, while still warm, onto a watch glass so it may cool. After cooling place the material, along with the other crystals of dibromobenzene, on a porous glass plate and press it to separate the acid. Add the pressed dibromobenzene to ethyl alcohol and recrystallize, it should now be quite pure. The hydrobromic acid that remains can be purified by fractional distillation. The fraction below 126 °C is water, which can be discarded. When the temperature reaches 126 and stays constant, begin collecting the distillate; this should be about 48% hydrobromic acid.

calcium carbonate			CaCO₃	CAS number 471-34-1
mp 825 (dec)	bp -	d 2.83	m 100.09	c $?.??
Safety Data: MSDS
Synonyms: aglime; aragonite; atomite; Calcichew; Calcidia; Calcit; calcite; carbonic acid calcium salt (1:1); chalk; Citrical; limestone; marble; slaker rejects; vaterite; whiting
Synthesis: Coming soon!

calcium chloride			CaCl₂	CAS number 10043-52-4
mp 772	bp 1600	d 2.152	m 110.98	c $?.??
Safety Data: MSDS Irritant
Synonyms: calcium dichloride; calcosan; intergravin-orales
Synthesis: Coming soon!

calcium hydroxide			Ca(OH₂)	CAS number 1305-62-0
mp -	bp -	d 2.08-2.34	m 74.09	c $?.??
Safety Data: MSDS Corrosive
Synonyms: calcium dihydroxide; calcium hydrate; carboxide; hydrated lime; lime, hydrated; lime water; slaked lime
Synthesis: Coming soon!