Ethanol → HCID 12895872, compound

Participants

Reaction Steps

To a mixture of 273 mg of 2-(10,11-dihydro-6-methoxy-11-oxodibenzo[b,f]thiepin-2-yl)-propionamide and 8 ml of ethanol was added 800 mg of potassium hydroxide in 2 ml of water, and the resulting mixture was refluxed with stirring for 6 hours. The solvent or ethanol was distilled off to obtain a residue, to which was added water, and the mixture was washed with benzene. 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 a yellowish-brown oil, which was chromatographed over 9 g silica gel and eluted with chloroform to obtain light yellow crystals. The crystals were recrystallized from benzene-n-hexane to obtain 165 mg (yield: 60%) of 2-(10,11-dihydro-6-methoxy-11-oxodibenzo-[b,f]thiepin-2-yl)-propionic acid as light yellow crystals having a melting point of 176°-178° C.

Provenance & Evidence