反应详情

10 ml. of anhydrous hydrazine was added to a solution of 10 g. of 7-chloro-2-(N-nitrosomethylamino)-5-phenyl-3H-1,4-benzodiazepine 4-oxide in 100 ml. of tetrahydrofuran and 50 ml. of methanol. After sitting at room temperature for 1 hour, the reaction mixture was evaporated under reduced pressure. The crystalline residue was partitioned between methylene chloride and water. The methylene chloride solution was dried and evaporated. Crystallization from methylene chloride/ether yielded 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine 4-oxide with a melting point of 290°-292° dec.

1. customthe reaction mixture was evaporated under reduced pressure
2. customThe crystalline residue was partitioned between methylene chloride and water
3. dry with materialThe methylene chloride solution was dried
4. customevaporated
5. customCrystallization from methylene chloride/ether