Sodium Hydroxide → HCID 20449976, compound

Participants

Reaction Steps

9 g of 1-bromo-8-chloro-6-(2-chlorophenyl)-4H-s-triazolo[4,3-a][1]benzazepine are stirred at 140° for 22 hours in 263 ml of 85% phosphoric acid. The mixture is poured on to 1.5 kg of ice water and neutralized with 28% sodium hydroxide solution. The product is extracted with chloroform. The residue from the chloroform extracts is chromatographed on 300 g of silica gel. Impurities are separated by elution with chloroform. By elution with chloroform which contains 2% or 4% ethanol, crystallization of the resulting material from diethyl ether/diisopropyl ether and recrystallization from ethyl acetate there is obtained 8-chloro-6-(2-chlorophenyl)-2,4-dihydro-1H-s-triazolo[4,3-a][1]benzazepin-1-one of melting point 250°-251°.

Provenance & Evidence