Sulfuric Acid → HCID 86736042, compound

Participants

Reaction Steps

To a mixture of 1.7 parts of 7-chloro-2-hydrazino-3-isobutyl-5-phenyl-3H-1,4-benzodiazepine prepared in Examples 8 and 11, 3.7 parts of triethyl orthoformate and 40 parts by volume of ethanol, is added 1 part of concentrated sulfuric acid with stirring and ice-cooling. The mixture is stirred for about 20 minutes at room temperature. After completion of reaction, the mixture is neutralized with sodium bicarbonate, followed by extraction with chloroform. The chloroform layer is washed with water and dried over sodium sulfate. After evaporation of the solvent, the residue is treated with n-hexane, whereby 8-chloro-4-isobutyl-6-phenyl-4H-s-triazolo [4,3-a][1,4] benzodiazepine is yielded as pale yellow crystals. Recrystallization from a mixture of benzene and n-hexane yields colorless needles melting at 140.5° C to 141.5° C.

Provenance & Evidence