Hydrochloric Acid → HCID 12895867, compound

Participants

Reaction Steps

A mixture of 200 mg of 2-(9-chloro-10,11-dihydro-11-oxodibenzo[b,f]thiepin-2-yl)-propionamide, 3 g of sodium hydroxide, 25 ml of water, 30 ml of methanol and 2 ml of tetrahydrofuran was refluxed for 14 hours. After the completion of the reaction, the solvent was removed by distillation to obtain a residue, to which was added water, and the mixture was acidified with with 10% hydrochloric acid and then extracted with chloroform. The extract was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain crystals, which were chromatographed over silica gel and eluted with chloroform. The thus obtained product was recrystallized from ethyl acetate to give 95 mg (yield: 48%) of 2-(9-chloro-10,11-dihydro-11-oxodibenzo[b,f]thiepin-2-yl)-propionic acid as light yellow crystals having a melting point of 163°-164° C.

Provenance & Evidence