Hydrochloric Acid → 5-(2-hydroxyethoxy)-7-chloro-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine

関与物質

反応手順

To a solution of 5-ethoxycarbonylmethoxy-7-chloro-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (2.2 g) in tetrahydrofuran (50 ml) is added with stirring lithium borohydride (0.28 g) at room temperature, and the mixture is refluxed for 30 minutes. The reaction solution is poured into diluted hydrochloric acid and extracted with dichloromethane. The extract is dried over magnesium sulfate and the solvent is distilled off under reduced pressure. The resulting residue is purified by silica gel column chromatography (eluent; dichloromethane:methanol=100:1→50:1), and recrystallized from dichloromethane/diethyl ether to give 5-(2-hydroxyethoxy)-7-chloro-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (1.6 g) as white powder, mp. 185°-187.5° C.

情報源と証拠