Ammonia → HCID 86736039, compound

Participants

Reaction Steps

A mixture of 1.98 parts of 7-chloro-2-(2-enanthylhydrazino)-5-phenyl-3H-1,4-benzodiazepine and 30 parts of polyphosphoric acid is heated at 170° C to 180° C for 2 hours. To the mixture is added 200 parts by volume of ice-water and the resulting solution is neutralized with concentrated aqueous ammonia under ice-cooling, followed by extraction with chloroform. The chloroform layer is washed with water, dried over sodium sulfate and the solvent is evaporated. The residue is recrystallized from aqueous acetone to yield 8-chloro-1-hexyl-6-phenyl-4H-s-triazolo [4,3-a] [1,4] benzodiazepine as colorless plates melting at 75° C to 78° C (sintering).

Provenance & Evidence