反应详情

1-Hydroxy-2-nitro-2-azapropane (0.52 g, 4.9 mmol) and acetonitrile (0.5 ml) were stirred under nitrogen at -20° C. as 2-nitro-2-azapropyl trifluoroacetate (1.09 g, 5.4 mmol) was added in one portion. The reaction flask was immediately connected to a vacuum pump and brought to 1-2 mm during several minutes. The reaction temperature was allowed to warm to ambient during 21/2 hours, a precipitate forming at about 10° C. After stirring an additional 11/2 hours, the vacuum was removed and cold ether (5 ml) was stirred with the solid mass 5 minutes before filtering bis(2-nitro-2-azapropyl) ether; yield: 0.83 g (87%); m.p. 30°-38.5° C. Recrystallization from ether gave bis(2-nitro-2-azapropyl) ether; yield: 0.55 g (58%); m.p. 38°-41° C. The analytical sample melted at 40.6°-42° C.

1. additionwas added in one portion
2. waitbrought to 1-2 mm during several minutes
3. temperatureto warm
4. custom2 hours
5. customa precipitate forming at about 10° C
6. customthe vacuum was removed
7. stirringcold ether (5 ml) was stirred with the solid mass 5 minutes
8. filtrationbefore filtering bis(2-nitro-2-azapropyl) ether
9. customRecrystallization from ether