反应详情

A mixture of 13.5 g. of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine 4-oxide, 200 ml. of ethanol, 9 ml. of triethylorthoacetate and 0.5 g. of p-toluenesulfonic acid was refluxed for 20 minutes. The ethanol was removed under reduced pressure. The residue was partitioned between methylene chloride and aqueous sodium carbonate solution. The methylene chloride layer was dried and evaporated. The remaining crystals were recrystallized from ethyl acetate to yield 8-chloro-1-methyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine 5-oxide with a melting point of 280°-282°.

1. additionA mixture of 13.5 g
2. customThe ethanol was removed under reduced pressure
3. customThe residue was partitioned between methylene chloride and aqueous sodium carbonate solution
4. dry with materialThe methylene chloride layer was dried
5. customevaporated
6. customThe remaining crystals were recrystallized from ethyl acetate