反应详情

Crude 3,3,5,7,7-pentanitro-5-azanonane-1,9-diol-1,9-diacetate (66.5 g) was stirred in 615 ml of warm (50° C.) MeOH in a 2000 ml round-bottom flask. Distilled water (265 ml) was added followed by 19 ml of concentrated hydrochloric acid. The mixture was heated at 67°-69° C. (mild reflux) overnight before nearly all the solvent was removed under reduced pressure on a rotary evaporator (water bath at 35° C.). The white solid (mp 118°-120° C.) was removed by filtration and washed with cold water. Crystallization from methanol-water gave 50.0 g, mp 121.5°-123° C. The second crop (2.9 g, mp 118°-120° C.) raised the yield to 52.9 g (97 percent). 1H NMR (acetone-d6 +1 dr. D2O): δ3.00 (t, 2H), 2.90 (t, 2H), 5.57 (s, 2H).

1. temperatureThe mixture was heated at 67°-69° C.
2. temperature(mild reflux) overnight before nearly all the solvent
3. customwas removed under reduced pressure on a rotary evaporator (water bath at 35° C.)
4. customThe white solid (mp 118°-120° C.) was removed by filtration
5. washwashed with cold water
6. customCrystallization from methanol-water
7. customgave 50.0 g, mp 121.5°-123° C
8. temperatureThe second crop (2.9 g, mp 118°-120° C.) raised the
9. customyield to 52.9 g (97 percent)