反应详情

To 50 mg of (5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]oxepin-8-yl)-acetamide was added 0.4 g of potassium hydroxide in 4 ml of water/ethanol (1:1), and the mixture was refluxed for 3 hours. After cooling, to this was added water, and the mixture was washed with ethyl acetate. The aqueous layer was acidified with acetic acid and extracted with ethyl acetate. The extract was washed with water and then a saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain a solid, which was recrystallized from acetone to give 37 mg (yield: 72%) of (5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]oxepin-8-yl)-acetic acid as white needle crystals having a melting point of 181°-184° C.

1. temperaturethe mixture was refluxed for 3 hours
2. temperatureAfter cooling
3. washthe mixture was washed with ethyl acetate
4. extractionextracted with ethyl acetate
5. washThe extract was washed with water
6. dry with materiala saturated sodium chloride solution and dried over anhydrous sodium sulfate
7. distillationThe solvent was distilled off
8. customto obtain a solid, which
9. customwas recrystallized from acetone