Sulfuric Acid → HCID 86736041, compound

Participants

Reaction Steps

To a mixture of 5.3 parts of 2-hydrazino-7-methyl-5-phenyl-3H-1,4-benzodiazepine prepared in Example 5, 14.8 parts of ethyl orthoformate and 150 parts by volume of ethanol, is added dropwise 4 parts of fconcentrated sulfuric acid under cooling. The whole mixture is stirred for about 30 minutes and neutralized with a saturated aqueous solution of 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-methyl-6-phenyl-4H-s-triazolo [4,3-a][1,4] benzodiazepine is yielded as crystals. Recrystallization from ethyl acetate yields pale yellow prisms melting at 177° C to 178° C.

Provenance & Evidence