Hydrochloric Acid → HCID 131715560, compound

Participants

Reaction Steps

A stirred suspension of (cis)-3-(hydroxy)-7-chloro-1-[3-(dimethylamino)propyl]-1,3,4,5-tetrahydro-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one, monohydrochloride (0.96 g; 2.18 mmol) in 35 ml of acetic anhydride was heated in an oil bath under argon and the resulting solution kept at 115°-118,° C. for 3 hours. The acetic anhydride was removed on a rotary evaporator at 0.2 mm to give a solid. The latter was rubbed under ethyl acetate, treated with 0.5 ml of saturated hydrogen chloride in ether to pH 2 and the evaporation repeated. The solid was rubbed under ether, evaporated, and pump-dried. The colorless material was rubbed under fresh ether, cooled overnight, filtered, washed with ether, and dried in vacuo; yield, 0.96 g; melting point 212°-215° C. (dec.), s, 200° C. TLC: Rf =0.32 (8:1:1, dichloromethane-methanol-acetic acid).

Provenance & Evidence