2-(2-ACETYLHYDRAZINO)-7-CHLORO-5-PHENYL-3H-1,4-BENZODIAZEPINE synthesis

Yield:-

Reaction Conditions:

in ethanol;dichloromethane

Steps:

A A.
A. 2-(2-acetylhydrazino)-7-chloro-5-phenyl-3H-1,4-benzodiazepine A mixture of 2.0 g. (0.0070 mole) of 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepine-2-thione, 1.55 g. (0.021 mole) of acetic acid hydrazide and 70 ml. of absolute ethanol was refluxed for 24 hours with a slow stream of nitrogen bubbling through the mixture. The mixture was then concentrated to give a residue. A suspension of this residue in methylene chloride was filtered. Concentration of the filtrate and crystallization of the residue from ethyl acetate gave 0.65 g. of 2-(2-acetylhydrazino)-7-chloro-5-phenyl-3H-1,4-benzodiazepine of melting point 196°-197° C. (dec.). The analytical sample of melting point 199°-200° C. (dec.) was prepared by recrystallizing some of this material from methylene chloride-ethyl acetate.

References:

The Upjohn Company US3987052, 1976, A