反应详情

A mixture of 11.7 parts of methyl 2-bromo-3-nitrobenzoate, 8.1 parts of 1,2-ethanediamine monohydrate and 40 parts of 1-butanol was stirred for 1/2 at reflux temperature. The reaction mixture was evaporated and the residue was diluted with 50 parts of water. The precipitate was filtered off and washed with water and 2-propanol. It was then recrystallized from 2-methoxyethanol, yielding 6.5 parts of 2,3,4,5-tetrahydro-9-nitro-1H-1,4-benzodiazepin-5-one; mp. 191°-195° C. (interm. 1).

1. temperatureat reflux temperature
2. customThe reaction mixture was evaporated
3. additionthe residue was diluted with 50 parts of water
4. filtrationThe precipitate was filtered off
5. washwashed with water and 2-propanol
6. customIt was then recrystallized from 2-methoxyethanol