1-Butanol → HCID 20449965, compound

Participants

Reaction Steps

12.1 g of 7-chloro-5-(2-fluorophenyl)-2-hydrazino-3H-1-benzazepine are heated to boiling under reflux for 2 hours in a mixture of 330 ml of n-butanol and 110 ml of triethyl orthoformate. The mixture is evaporated in vacuo. The residue is crystallized from hexane, there being obtained crude 8-chloro-6-(2-fluorophenyl)-4H-s-triazolo[4,3-a][1]benzazepine as reddish coloured crystals. This material is purified by chromatography on 121 g of silica gel. Impurities are eluted with benzene/methanol (99:1). The product is subsequently eluted with benzene/methanol (98.5:1.5 and 98:2). After crystallization of the resulting material from ether, there is obtained 8-chloro-6-(2-fluorophenyl)-4H-s-triazolo[4,3-a][1]benzazepine of melting point 180°-182°.

Provenance & Evidence