Azane;hydrate → HCID 20338060, compound

Participants

Reaction Conditions

Reaction Steps

The mixture of 1.3 g of 2-[3'-(α-cyanoethyl)-phenoxy]-3-pyridylacetic acid and 30 g of polyphosphoric acid was stirred at 150° C. for 2 hours. After cooling, to this was added ice-water and the mixture was alkalified with 10% ammonia water and 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 the oil, which was chromatographed over silica gel, eluted with chloroform/ethanol (50/1), and there was obtained a solid substance. This was recrystallized from methanol to give 250 mg of 2-(5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]oxepin-9-yl)-propionamide as pale yellow powder having a melting point of 89°-90° C.

Provenance & Evidence