反应详情

温度

-60 °C

A suspension/solution of 100 mmoles of N2O5 in 175 ml. of CH2Cl2 was prepared by ozonolysis of N2O4 at -60° C. This suspension was diluted by adding 60 ml. of CH3CN, cooled to -78° C., and 100 mmoles (13.7 grams) of the ammonium N(methoxycarbonyl)N-nitro-amide (ammonium N-nitromethylcarbamate) made in Example IV was added to the reaction mixture. The mixture was then stirred for 1 hour while it was allowed to slowly warm to -60° C. over that hour. Excess ammonia gas was then added until the pH reached 9. A thick precipitate developed. The reaction mass was concentrated in vacuo in a rotary evaporator, and 100 ml. of CH3CN and 100 ml. of ethylacetate were then added. The reaction mixture was then filtered and then washed with ethylacetate. The filtrate was then concentrated to approximately 30 ml. and 200 ml. of CHCl3 was then added to precipitate the product from the filtrate. The solid ammonium dinitramide product was then filtered and collected. The product was then dried in vacuo to yield 6.4 grams (52%) of ammonium dinitramide salt.

1. additionThis suspension was diluted
2. additionby adding 60 ml
3. additionwas added to the reaction mixture
4. concentrationThe reaction mass was concentrated in vacuo in a rotary evaporator, and 100 ml
5. additionof ethylacetate were then added
6. filtrationThe reaction mixture was then filtered
7. washwashed with ethylacetate
8. concentrationThe filtrate was then concentrated to approximately 30 ml
9. additionof CHCl3 was then added
10. customto precipitate the product from the filtrate
11. filtrationThe solid ammonium dinitramide product was then filtered
12. customcollected
13. customThe product was then dried in vacuo