反应详情

To a solution of 0.25 part of 2-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine in 8 parts by volume of methanol is added 0.2 part by volume of hydrazine hydrate (100%) with stirring and the stirring is continued at room temperature for further 2.5 hours. To the reaction mixture is added water, followed by extraction with chloroform. Chloroform layer is washed with water and dried over anhydrous sodium sulfate, followed by distillation of the solvent. Treatment of the residue with n-hexane gives 2-hydrazino-7-nitro-5-phenyl-3H-1,4-benzodiazepine as orange crystalline powder. The product is treated with acetone, whereupon 2-(2-isopropylidenehydrazino)-7-nitro-5-phenyl-3H-1,4-benzodiazepine is obtained as pale yellow crystals melting at 203°-205° C.

1. extractionfollowed by extraction with chloroform
2. washChloroform layer is washed with water
3. dry with materialdried over anhydrous sodium sulfate
4. distillationfollowed by distillation of the solvent