Acetic Acid → HCID 20338036, compound

Participants

Reaction Steps

An amount of 50 mg of 2-(5,6-dihydro benzo[b]pyrido[3,2-f]-thiepin-8-yl)-propionic acid was dissolved in the mixed solvents of 20 ml of methylene chloride and 20 drops of chloroform by heating, and to this were added 50 mg of dicyclohexylcarbodiimide with ice-cooling, then dropwise 3 ml of methylene chloride saturated with liquid ammonia. The resulting mixture was stirred for 1.5 hours under a stream of nitrogen. After the completion of the reaction, to the mixture were added pieces of ice and acetic acid and the resulting mixture was extracted with chloroform. The extract was washed with saturated sodium hydrogencarbonate solution, then saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain the residue, which was chromatographed over silica gel, eluted with n-hexane/acetone (4/1-1/1), and there was obtained colorless solid. This was recrystallized from ethyl acetate to give 38 mg of 2-(5,6-dihydro benzo[b]pyrido[3,2-f]-thiepin-8-yl)-propionamide as colorless crystals having a melting point of 173.5°-175° C.

Provenance & Evidence