Acetic Acid → HCID 12895874, compound

Participants

Reaction Conditions

Reaction Steps

To a mixture of 300 mg of 2-(10,11-dihydro-7-fluoro-11-oxodibenzo[b,f]thiepin-2-yl)-propionamide and 3 ml of acetic acid was added 3 ml of hydrochloric acid, and the resulting mixture was stirred at 100° C. for 2 hours. After cooling, to this was added water, and the mixture was extracted with ethyl acetate. The extract was re-extracted with a dilute sodium hydroxide solution. The aqueous layer was acidified with hydrochloric acid and extracted with ethyl acetate. The extract was washed with a saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was removed by distillation to obtain yellow crystals, which were recrystallized from benzene, thereby obtaining 200 mg (yield: 67%) of 2-(10,11-dihydro-7-fluoro-11-oxodibenzo[b,f]thiepin-2-yl)-propionic acid as colorless crystals having a melting point of 147.5°-148° C.

Provenance & Evidence