Precursors Part 3


infusorial earth No Formula CAS number 61790-53-2
mp - bp - d - m - c $?.??
Safety Data: MSDS
Synonyms: Celite; diatomaceous earth; fossil flour; kieselguhr; siliceous earth; Super-Cel
Synthesis: Coming soon!

iodine I2 CAS number 7553-56-2
mp 113.60 bp 185.24 d 4.93 m 126.945 c $?.??
Safety Data: MSDS Corrosive
Synonyms:
Synthesis: Coming soon!

iron XaYbZc CAS number 7439-89-6 Fe
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

isopropyl alcohol CH3CHOHCH3 CAS number 67-63-0
mp -88.5 bp 82.5 d 0.78084 m 60.10 c $?.??
Safety Data: MSDS Flammable
Synonyms: 2-propanol; alcojel; alcosolve; alcosolve 2; avantin; chromar; combi-schutz; dimethylcarbinol; hartosol; 2-hydroxypropane; imsol a; IPA; i-propanol; isohol; isopropanol; lutosol; petrohol; propan-2-ol; n-propan-2-ol; propol; rubbing alcohol; sec-propanol; sec-propyl alcohol; spectrar; sterisol hand disinfectant; takineocol
Synthesis: Coming soon!

isopropylamine (CH3)2CHNH2 CAS number 75-31-0
mp -101 bp 33-34 d 0.694 m 59.11 c $?.??
Safety Data: MSDS
Synonyms: 2-propanamine; 2-aminopropane; monoisopropylamine; propan-2-amine; sec-propylamine
Synthesis: Nothing yet

lead acetate Pb(CH3COO2) CAS number 301-04-2
mp 75 bp 100 dec d 2.55 m 325.29 c $?.??
Safety Data: MSDS Toxic
Synonyms: acetic acid, lead(2+) salt; dibasic lead acetate; lead diacetate; lead dibasic acetate; lead(II) salt acetic acid; neutral lead acetate; normal lead acetate; salt of Saturn; sugar of lead
Synthesis: Coming soon!

lead monoxide PbO CAS number 1317-36-8
mp 888 bp ? d 9.53 m 223.20 c $?.??
Safety Data: MSDS Toxic
Synonyms: C.I. 77577; lead ocher; lead oxide; lead (II) oxide; lead oxide (mono); lead oxide yellow; lead protoxide; litharge; litharge yellow L-28; massicot; Massicotite; pigment yellow 46; plumbous oxide; yellow lead ocher
Synthesis: Coming soon!

lead nitrate Pb(NO3)2 CAS number 10099-74-8
mp ? bp ? d 4.53 m 331.21 c $?.??
Safety Data: MSDS Oxidizer, Toxic
Synonyms: lead dinitrate; lead (II) nitrate; nitric acid, lead(2+)salt
Synthesis: Coming soon!

magnesium oxide MgO CAS number 1309-48-4
mp 2800 bp ? d ? m 40.30 c $?.??
Safety Data: MSDS
Synonyms: calcined brucite; calcined magnesia; Irtran-5; Magcal; Maglite; magnesia; magnesia usta; magnesium monoxide; magnesium oxide, heavy; magnesium oxide, light
Synthesis: Coming soon!

magnesium styphnate XaYbZc CAS number 13255-27-1
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

maltose C12H22O11 CAS number 69-79-4 and 16984-36-4
mp 103 bp ? d ? m 342.30 c $?.??
Safety Data: MSDS
Synonyms: 4-O-alpha-D-glucopyranosyl-D-glucose; 4-(alpha-D-glucosido)-D-glucose; maltobiose; Maltos; alpha-maltose; D-(+)-maltose; malt sugar; Martos-10
Synthesis: Nothing yet

mannitol C6H14O6 CAS number 87-78-5 and 69-65-8
mp 166-168 bp 290-295 d 1.52 m 182.17 c $?.??
Safety Data: MSDS
Synonyms: cordycepic acid; Diosmol; Manicol; manna sugar; Mannidex; mannite; D-mannitol; Osmitrol; Osmosal; Resectisol
The listed boiling point is at 3.5 mm of Hg Synthesis: Nothing yet

mercuric nitrate Hg(NO3)2 CAS number 10045-94-0
mp 79 bp ? d ? m 324.60 c $?.??
Safety Data: MSDS Toxic
Synonyms: mercury nitrate; mercury (II) nitrate; mercury pernitrate; nitric acid, mercury salt
Synthesis: Coming soon!

mercuric oxide HgO CAS number 21908-53-2
mp 500 dec bp - d 11.14 m 216.59 c $?.??
Safety Data: MSDS Toxic
Synonyms: mercury oxide; red mercury (II) oxide; Santar; yellow mercury (II) oxide; yellow oxide of mercury
Synthesis: Coming soon!

mercury Hg CAS number 7439-97-6
mp -38.87 bp 356.72 d 13.534 m 200.59 c $?.??
Safety Data: MSDS Toxic
Synonyms: hydrargyrum; liquid silver; Marcero; quick silver; Rathje
Synthesis: Coming soon!

methenamine C6H12N4 CAS number 100-97-0
mp 263 dec bp - d ? m 140.19 c $?.??
Safety Data: MSDS
Synonyms: 1,3,5,7-tetraazatricyclo[3.3.1.13,7]decane; aceto hmt; Aminoform; Ammoform; ammonioformaldehyde; Cystamin; Cystogen; formamine; Formin; HEXA; Hexaform; hexamethylenamine; hexamethyleneamine; hexamethylenetetraamine; hexamethylene tetramine; hexamethylene triamine; hexamine; hexilmethylenamine; Hiprex; HMT; HMTA; Mandelamine; methamin; metheneamine; preparation af; resotropin; 1,3,5,7-tetraazaadamantane; tetraazatricyclo[3.3.1.1(3,7)]decane; UREX; Uritone; Uroqid; Urotropin
Synthesis: Nothing yet

3-methoxy-2,2',4,4',6,6'-hexanitrobiphenyl XaYbZc CAS number 51776-63-7
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

2-methoxy-2-methyl-4,5-imidazolidinedione C5H8N2O3 CAS number 214191-56-7
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: This substance is used to prepare the explosive FOX-7. I don’t know how long this stuff will sit around, so it may be wise to prepare it shortly before its intended use.
     Preparation of 2-methoxy-2-methyl-4,5-imidazolidinedione. Prepare a solution of 69.6 g of sodium methoxide in 1100 mL of methyl alcohol in a 2-L round bottomed flask. Add a magnetic stir bar to the flask and set it up for stirring. While stirring, add 36.48 g of acetamidine hydrochloride to the flask and keep stirring until a well mixed suspension forms. Prepare a second solution of 55.88 g of diethyl oxalate in 400 mL of methyl alcohol. Attach an addition funnel to the flask and slowly add the diethyl oxalate solution drop by drop over a period of 3 hours. Maintain stirring throughout the addition. After the addition is complete remove the addition funnel and set up a cold water bath for the flask. Insert a thermometer in the flask and slowly add enough concentrated hydrochloric acid to lower the pH of the mixture to 9 while keeping the temperature below 30 °C. Use the cold water bath as necessary to lower the temperature.
     At this point a precipitate of sodium chloride should have formed. Pour the contents of the flask over a filter to remove this solid. The salt collected on the filter paper can be discarded. Pour the liquid filtrate back into the flask and set the flask up for a simple distillation. Very gently heat the flask to distill off the methyl alcohol. This alcohol should be fairly pure and can be recycled. In this situation the flask is distilled to dryness to remove all alcohol and leave a solid white powder. When very little alcohol remains reduce the heat to around 30 degrees until dry. At this point this is a mixture of waste sodium chloride, 2-methyl-4,5-imidazoledione and our final product. Heat a beaker of 320 mL of methyl alcohol to boiling and add it to the flask with the solid. Allow a few minutes for the soluble portions to dissolve and immediately filter the liquid while still hot to remove any insoluble impurities. Again this is just salt, which can be discarded and the liquid kept. Redistill this liquid until a volume of only 320 mL remains, and then place the liquid in a refrigerator to cool overnight. This process will convert the 2-methyl-4,5-imidazoledione to the final product. In the morning a white crystalline material should have precipitated in the bottom of the flask. Filter this liquid to collect the crystals and allow them to dry. The crystals should be 2-methoxy-2-methyl-4,5-imidazolidinedione with a yield around 64% or 35-36 g.

methyl acrylate CH2=CHCOOCH3 CAS number 96-33-3
mp -76.5 bp ? d 0.9561 m 86.09 c $?.??
Safety Data: MSDS
Synonyms: 2-propenoic acid methyl ester; acrylic acid methyl ester; curithane 103; methoxycarbonylethylene; methyl ester acrylic acid; methyl propenoate; methyl 2-propenoate; propenoic acid methyl ester
Synthesis: Nothing yet

methyl alcohol CH3OH CAS number 67-56-1
mp -97.8 bp 64.7 d 0.7866 m 32.04 c $?.??
Safety Data: MSDS Flammable, Toxic
Synonyms: carbinol; colonial spirit; columbian spirits; methanol; methyl hydroxide; methylol; monohydroxymethane; pyroxylic spirit; wood; wood alcohol; wood naphtha; wood spirit
Synthesis: Nothing yet

methylamine CH3NH2 CAS number 74-89-5
mp -93.5 bp -6.3 d 0.699 m 31.06 c $?.??
Safety Data: MSDS Flammable, Irritant
Synonyms: aminomethane; carbinamine; methanamine; mercurialin; monomethylamine
Synthesis:    Prepare a solution of 25 g of dried acetamide and 23 mL of bromine in a 500-mL flask. Place the flask into a cold water bath. Gradually add a solution of 40 g of potassium hydroxide in 350 mL of water to the flask until the brownish red color turns to bright yellow, some hydroxide solution may remain unused. This mixture is then added to a 1-L flask containing a solution of 80 g of potassium hydroxide in 150 mL of water heated to 70-75 °C. The addition should be done by an addition funnel in a continuous stream over the course of 2-3 minutes. The liquid is maintained at 70-75 °C until it becomes colorless, this will take approximately 15-30 minutes. If at any time the temperature rises above 75 °C, the flask must be cooled by immersion for a short time in cold water.
     The methylamine that should have formed is then removed by steam distillation; it is collected in a receiver containing a mixture of 52 mL of concentrated hydrochloric acid and 40 mL of water. To insure that the methylamine is completely absorbed by the acid, it must be bubbled into the receiver straight from the condenser. If you are using a vacuum adapter to direct the flow of liquid into the receiver, attach a piece of glass tubing to the tip so it extends to the bottom of the receiver. Otherwise, just connect a one-hole stopper to the condenser with an angled piece of glass tube extending into the bottom of the receiver. Make sure the tube end in the condenser is near the bottom of the stopper, not the middle, so the condensed liquid can drain easier. Periodically test the pH of the condensed liquid, when it is no longer basic discontinue the distillation.
     The resulting methylamine hydrochloride is partially evaporated in a porcelain dish heated over a flame, then to dryness by heating on a water bath. It is finally heated on a hotplate to 100 °C until it is dry and dusty. The crude methylamine thus obtained is contaminated with some ammonium chloride salt. Grind the dried substance into a fine powder followed by recrystallization from 100% ethyl alcohol. Filter to collect the crystals, and then dry them in a desiccator.

methylene chloride CH2Cl2 CAS number 75-09-2
mp -95 bp 39.75 d 1.3255 m 84.93 c $?.??
Safety Data: MSDS
Synonyms: dichloromethane; Aerothene MM; DCM; Freon 30; methane dichloride; methylene bichloride; methylene dichloride; narkotil; R 30; Refrigerant 30; solaesthin; solmethine
Synthesis: Nothing yet

2-methyl-2-nitro-1,3-propanediol C4H9NO4 CAS number 77-49-6
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms: 2-methyl-2-nitropropane-1,3-diol; 2-nitro-2-methyl-1,3-propanediol; NMPD
Synthesis: Nothing yet

2-methyl-2-nitro-1-propanol C4H9NO3 CAS number 76-39-1
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms: 2-methyl-2-nitropropanol; 2-nitro-2-methylpropanol; 2-nitro-2-methyl-1-propanol
Synthesis: Nothing yet

metriol XaYbZc CAS number 77-85-0
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

naphthalene C10H8 CAS number 91-20-3
mp 80.2 bp 217.9 d 1.162 m 128.17 c $?.??
Safety Data: MSDS
Synonyms: camphor tar; mighty 150; mighty rd1; mothballs; moth flakes; naphthanin; naphthene; tar camphor; white tar
Synthesis: Coming soon!

3-nitrazabutylamine XaYbZc CAS number ?
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

nitric acid HNO3 CAS number 7697-37-2
mp -41.59 bp 83 d 1.4134-1.5129 m 63.01 c $?.??
Safety Data: MSDS Corrosive, Oxidizer
Synonyms: aqua fortis; azotic acid; fuming nitric acid; hydrogen nitrate; Nital; nitric acid red fuming; nitryl hydroxide; red fuming nitric acid; Rfna; Salpetersäure
Synthesis: The densities listed are for 70% and 100% acid. A density of up to 1.544 can be reached with 12.7% dissolved nitrogen dioxide in fuming nitric acid. Nitric acid forms an azeotrope with water at 68%, it this has a bp of 120.5 °C (yes, this bp is higher than either water or the acid boils at pure).

nitric oxide NO CAS number 10102-43-9
mp - bp -151.8 d - m 30.01 c $?.??
Safety Data: MSDS
Synonyms: mononitrogen monoxide; nitrogen monoxide; nitrogen oxide; NO
Synthesis: Nothing yet

nitroallyl acetate XaYbZc CAS number 1794-92-9
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

m-nitroaniline C6H6N2O2 CAS number 99-09-2
mp 114 bp 306 d 0.9011 m 138.13 c $?.??
Safety Data: MSDS
Synonyms: 3-nitrobenzenamine; amarthol fast orange r base; m-aminonitrobenzene; 1-amino-3-nitrobenzene; azobase mna; C.I. 37030; C.I. azoic diazo component 7; daito orange base r; devol orange r; diazo fast orange r; fast orange base r; fast orange m base; fast orange mm base; fast orange r base; hiltonil fast orange r base; naphtoelan orange r base; nitranilin; m-nitraniline; m-nitroaminobenzene; 3-nitroanaline; 3-nitroaniline; m-nitrophenylamine; orange base irga 1
Synthesis:    Dissolve 10 g of m-dinitrobenzene in 40 mL of ethyl alcohol in a round-bottomed 250-mL Florence flask. Place the flask into a salt-ice bath to cool it down; some dinitrobenzene should separate out. The solution is then treated with 9 mL of 27-30% ammonium hydroxide. You must use only concentrated ammonium hydroxide, adding extra dilute hydroxide will not work in this case. Remove the flask from the ice bath and allow it to warm to room temp before proceeding with the next step.
     For the synthesis to be most effective it is necessary to weigh the flask (that includes the contents of the flask), the following reaction is complete when the weight of the flask has increased by 6 g. Saturate the mixture in the flask by bubbling in hydrogen sulfide gas; stop when it appears no more is being absorbed. The saturated mixture is now refluxed for 30 minutes. Allow the flask to cool to room temperature, and again saturate the mixture with hydrogen sulfide, followed by refluxing. Continue the process of saturating and refluxing until the weight increase of 6 g is achieved. Without a scale it will be difficult to judge when to stop, some experimentation will be necessary on your Part.
     The mixture is now diluted with water, the resulting precipitate is collected on a filter, washed with water, and extracted several times by warming with dilute hydrochloric acid. The acidic extractions now contain the nitroaniline, it can be precipitated by neutralizing the liquid with ammonium hydroxide. The crystals are collected by filtration, and then recrystallized from water. The yield is about 70-80%.

nitrobenzene C6H5NO2 CAS number 98-95-3
mp 6 bp 210-211 d 1.205 m 123.11 c $?.??
Safety Data: MSDS Toxic
Synonyms: essence of mirbane; essence of myrbane; mirbane oil; nitrobenzol; oil of mirbane; oil of myrbane
Synthesis:    Prepare a mixture of 82 mL of 95-100% sulfuric acid and 71 mL of 70% nitric acid in a 500-mL flask. Stir well and allow the mixture to cool to room temperature in a cold water bath. Gradually add 57 mL of benzene to the acid with frequent shaking. If the temperature rises above 50-60 °C during the benzene addition, stop adding benzene and cool the flask in a cold water bath until the temperature has lowered. After all of the benzene has been added, reflux the flask in a water bath at 60 °C for 1 hour. The temperature of the water bath should be 60 °C, not the contents of the flask. Shake the flask frequently during reflux.
     After heating, allow the flask to cool, two layers should form. Transfer the contents to a separatory funnel and drain off the bottom layer of sulfuric and nitric acids; the top layer contains the nitrobenzene. The bottom layer can be disposed of. The nitrobenzene is then vigorously shaken in the separatory funnel several times with water. After each shaking, allow the layers to separate, the nitrobenzene will now be the bottom layer, dispose of the top water layer. After washing, place the nitrobenzene in a dry Erlenmeyer flask with some calcium chloride. Heat this flask on a steam bath, it will first be milky, then it will go clear, stop when it is clear. The nitrobenzene is now purified by simple distillation. Yield is about 60-70 g.

2-nitro-2-(3',5'-dinitrophenyl)-propanediol-1,3 XaYbZc CAS number ?
mp ? bp ? d ? m ? c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Nothing yet

nitroethane CH3CH2NO2 CAS number 79-24-3
mp -50 bp 114-115 d 1.041 m 75.07 c $?.??
Safety Data: MSDS
Synonyms: nitroetan
Synthesis: Nothing yet

nitrogen N2 CAS number 7727-37-9
mp -210.01 bp -195.79 d - m 28.0134 c $?.??
Safety Data: MSDS
Synonyms:
Synthesis: Coming soon!

nitrogen dioxide NO2 CAS number 10102-44-0
mp -9.3 bp 21.15 d 1.448 m 46.01 c $?.??
Safety Data: MSDS
Synonyms: nitrogen oxide; nitrogen peroxide; NO2
Synthesis: This is made accidently or as a waste product, I only listed it here because its so dangerous. You should know how to avoid making this, as well as how to deal with it if you do.

nitromethane CH3NO2 CAS number 75-52-5
mp -29 bp 101.2 d 1.1322 m 61.04 c $?.??
Safety Data: MSDS
Synonyms: nitrocarbol; NM
     Because nitromethane is useful as an explosive ingredient, its availability has dried up on the OTC market. One of its biggest uses is as automotive fuel for drag racers, they burn 100% anhydrous fuel instead of gasoline, but at $25 a gallon or more it's gonna cost ya. This is the same stuff used in the bomb at Oklahoma City, and McVeigh tipped off the feds asking for it at a drag race. It is also available as a component in fuel for model cars and airplanes at hobby shops, from which it can be distilled. Those fuels can be very expensive, however. Hobby shops usually sell it as high as 70% with other contaminants in it; they are also wise to someone asking for "the highest concentration of nitromethane" you should know exactly what kind of car you need the fuel for if you ask. To avoid the hassles of buying this forbidden fuel, I suggest making it yourself.
Synthesis:    Prepare a mixture of 500 g of chloroacetic acid and 500 g of crushed ice in a large beaker. Add to this enough cold 40% sodium hydroxide solution to neutralize the acid and make the pH of the solution slightly alkaline, about 360 mL should suffice. Do not allow the temperature to rise above 20 °C while adding the hydroxide, failing to do so will cause unwanted sodium glycolate to form. Prepare a solution of 365 g of sodium nitrite in 500 mL of water. Add this solution to the previous solution in a round bottom 3-L Florence flask.
     Set the flask up for simple distillation with the thermometer dipping into the liquid (yes, in the liquid, not at the condenser opening like it usually is). Keep the receiving flask cold with an ice water bath. Gently heat the solution until bubbles of carbon dioxide are evolved, this should happen at around 80 °C. Remove the heat as the reaction should proceed spontaneously, it should rise to around 100 °C while the nitromethane/water azeotrope distills over at 90 °C. If the temperature does not rise on its own, gently heat the flask to 85°C until it does. At this temperature the exothermic decomposition of the reactants becomes so rapid that continued application of heat might cause violent frothing, with significant loss of nitromethane. After the reaction subsides to 95-100°C, cautiously heat the flask to 110 °C, stop when no more nitromethane distills over.
     This should make about 130 mL of nitromethane with 370 mL of water, they should form separate layers. Place the layers into a separatory funnel and allow them to stand for 30 minutes, afterwards drain off the lower layer of nitromethane. The water layer is mixed with one fourth its weight of salt and distilled to give another 10-12 mL of nitromethane. Add this to the nitromethane already distilled. The crude nitromethane is dried over anhydrous calcium chloride in a desiccator and redistilled to give 115-125 mL of pure nitromethane.
     Yield is about 38%. The yield can be improved slightly by using 625 g of chloroacetic acid and 450 mL of 40% sodium hydroxide solution. Another increase in yield can be achieved by adding 374 g of boric acid after adding the sodium nitrite solution, but before doing any heating. You can use a smaller flask and do several distillations if you do not have a 3-L flask, just remember to never fill it more than two-thirds of the way.

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Megalomania's Controversial Chem Lab ©1997-2005 /synthesis3/ revised December 3, 2004