Potassium Hydroxide → HCID 20506969, compound

Participants

Reaction Steps

To 101 mg of 2-(5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]-thiepin-8-yl)-propionamide were added 0.4 g of potassium hydroxide, 1 ml of water and 4 ml of ethanol and the mixture was refluxed with stirring for 5 hours. After cooling, to this were added water and 3% sodium hydroxide solution, then a small amount of diethyl ether, and the mixture was shaked. The aqueous layer was collected and acidified with acetic acid, and to this was added sodium chloride, and the resulting mixture was extracted with chloroform. The extract was washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain 115 mg of brown glutinous substance, which was chromatographed over silica gel, eluted with chloroform/methanol(100/1-20/1), and there was obtained 83 mg of 2-(5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]thiepin-8-yl)-propionic acid as colorless glutinous substance. This was solidified by washing with n-hexane and there was obtained colorless crystals having a melting point of 141°-143° C.

Provenance & Evidence