Synthesis 1:
Into a 250 mL Erlenmeyer flask combine 3 g of potassium dinitramide and 3 g of finely powdered ammonium sulfate.  Add 100 mL of isopropyl alcohol and heat the flask, while stirring, until all of the solids dissolve.  Place the flask in a cold water bath to precipitate the byproduct of potassium sulfate.  Filter to remove the crystals of sulfate and gently heat the filtrate to concentrate it to a fraction of its volume.  Pour the concentrate into a beaker containing an excess of petroleum ether to precipitate ammonium dinitramide.  Filter to collect the crystals and dry them in an oven at 50 C.

Synthesis 2:
Prepare a mixture of 7.5 g of ammonium N-nitrourethane suspended in 200 mL of methylene chloride.  Cool this mixture to -50 C in an acetone-dry ice bath.  Prepare a second mixture of 45 mL of dinitrogen tetroxide in 200 mL of dry methylene chloride.  Cool this mixture to -78 C in an acetone-dry ice bath.  Bubble ozone into the second mixture, while stirring, until it is a dark blue color.  While bubbling the ozone allow the mixture to warm up to -30 C.  The mixture will now consist of dinitrogen pentoxide in methylene chloride.

Combine the two mixtures and let them sit for 1 hour.  During this time the temperature of the reaction mixture is allowed to warm to -30 C.  Bubble ammonia gas into the mixture to raise the pH to 10.  Filter to collect any insoluble material and add it to a beaker containing 150 mL of acetonitrile.  Stir the acetonitrile mixture for 20 minutes before filtering to remove any remaining undissolved impurities.

The filtrate is poured into a 4”x1” column containing 230-400 mesh silica gel.  The ammonium dinitramide is eluted by adding acetonitrile.  The resulting eluted filtrate is concentrated to 30 mL and treated with 30 mL of chloroform to precipitate pure ammonium dinitramide.  The crystals are filtered to collect them and allowed to dry.  Final yield is about 4 g or 60%.

Synthesis 3:
Prepare a mixture of 8.8 g of hydrofluoric acid and 40 g of ethylnitrate in 300 mL of dry nitromethane.  Place this mixture in a salt-ice bath and cool to 10 C.  Slowly add 100 g of boron trifluoride to the mixture while keeping the temperature between 10 and 15 C.  A few minutes after the addition filter to collect the crystals of nitronium tetrafluorate that form.  Wash the crystals with two 400 mL portions of a 1:1 mixture of methylene chloride and nitromethane, and then with one 400 mL portion of methylene chloride.

Place the nitronium tetrafluorate crystals into a beaker containing 400 mL of methylene chloride.  Cool the contents to -78 C in an acetone-dry ice bath.  Bubble 35 g of anhydrous ammonia into the beaker over a period of 2 hours while stirring.  Continue stirring the mixture for 12 hours while allowing it to warm to room temperature.  Filter to collect the solid material and wash it with 400 mL of methylene chloride.  Add the crystals to 150 mL of acetone and stir for 1 hour.  Add 150 mL of ethyl acetate to the mixture and filter to remove any undissolved material.  Gently heat the filtrate solution to dryness to obtain crude ammonium dinitramide.  The ammonium dinitramide can be purified by recrystallizing from n-butanol.  Final yield is about 5.5 g or 21%.

While a good faith effort has been made to ensure the accuracy of all scientific information presented on this page, the possibility exists that some errors have invaded the machine. Furthermore, there may be certain omissions of physical properties, reaction conditions, necessary equipment, storage and handling requirements, and critical safety data. As with any scientific endeavor, especially chemistry, the necessary safety precautions should be observed at all times.

I do not allow errors to persist on my website once they have been discovered, but I need your help to find them. If you observe an error in any procedure, or a critical omission of essential safety precautions, and you have a valid reference that I can independently verify to back up your claim, please contact me via the error reporting form. If there are omissions in this procedure, such as a missing boiling point, density, etc., please contact me if you can fill in the blanks. I am also interested in receiving any alternate methods, or improvements in the procedure to synthesize this compound. If you are interested in submitting your own information please use the user submission area.

If you have comments, additions, clarifications, or observations that you wish to add about this compound and its method of synthesis, post them on The Forum using the thread below . You must be a registered member of The Forum to make posts, which is free and easy to do. The rules of this commenting thread are different from the regular rules of The Forum. This thread is for additions to this page only, no questions or remarks are allowed that do not contribute to the scientific information of this compound are allowed. To that end all posts to this thread will be moderated.