反应详情

22.8 g Ethyl 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]-benzodiazepine-3-carboxylate were suspended under stirring and argon atmosphere in 91.2 ml 1,4-dioxane. 14.1 ml Formamide and 13.9 ml sodium methanolate were successively added to yield a clear light-orange solution, which turned to a white suspension after 10 minutes. This suspension was stirred two hours at 30° C. 200 ml Deionized water were added in one portion and 1,4-dioxane was distilled off at 40° C. under reduced pressure. The remaining white suspension was stirred two hours at 0° C. and filtered. The precipitate (7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide) was washed with 50 ml deionized water three times and dried under reduced pressure for 18 hours at 80° C. Crude product:19.43 g as a white powder. m.p. >250° C.

1. customto yield a clear light-orange solution, which
2. stirringThis suspension was stirred two hours at 30° C
3. distillationwas distilled off at 40° C. under reduced pressure
4. stirringThe remaining white suspension was stirred two hours at 0° C.
5. filtrationfiltered
6. washThe precipitate (7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide) was washed with 50 ml
7. customdried under reduced pressure for 18 hours at 80° C