反应详情

A mixture of 40 mg of (5,6-dihydro benzo[b]pyrido[3,2-f]-oxepin-8-yl)-acetic acid, 60 mg of dicyclohexylcarbodimide and 2 ml of dry dichloromethane was stirred under ice cooling. To the resulting mixture was added 8 ml of a saturated liquid ammonia-dichloromethane solution, and the mixture was stirred for 3 hours. After the completion of the reaction, this was basified with a saturated sodium hydrogen carbonate solution and extracted with ethyl acetate. The extract was washed with water and then with a saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain a light yellow oil, which was chromatographed over 4 g of silica gel and eluted with chloroform/ethyl acetate (10/1-8/2) to obtain crystals. These were recrystallized from ethyl acetate to yield 15 mg (yield: 40%) of (5,6-dihydro benzo[b]pyrido[3,2-f]oxepin-8-yl)-acetamide as light yellow needle crystals having a melting point of 164°-165° C.

1. stirringthe mixture was stirred for 3 hours
2. customAfter the completion of the reaction
3. extractionextracted with ethyl acetate
4. washThe extract was washed with water
5. dry with materialwith a saturated sodium chloride solution and dried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off
7. customto obtain a light yellow oil, which
8. customwas chromatographed over 4 g of silica gel
9. washeluted with chloroform/ethyl acetate (10/1-8/2)
10. customto obtain crystals
11. customThese were recrystallized from ethyl acetate