Methanol → HCID 12895880, compound

Participants

Reaction Steps

To a mixture of 78 mg of methyl 2-(8-amino-10,11-dihydro-11-oxodibenzo[b,f]thiepin-2-yl)-propionate and 3 ml of methanol was added with ice cooling 200 mg of potassium hydroxide in 3 ml of water, and the resulting mixture was stirred at room temperature for 6 hours. After filtrating the reaction mixture to remove insoluble substances, the filtrate 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 yellow solid substance, which was chromatographed over 2 g of silica gel and eluted with chloroform/methanol (50/1), and there were obtained yellow crystals. The thus obtained crystals were recrystallized from chloroform-methanol to obtain 49 mg (yield: 75%) of 2-(8-amino-10,11-dihydro-11-oxodibenzo[b,f]thiepin-2-yl)-propionic acid as light yellow crystals having a melting point of 189°-191° C.

Provenance & Evidence