反应详情

To a mixed solution of 6 ml of 4N hydrochloric acid and 6 ml of acetic acid was added 3.00 g of ethyl 8-chloro-1-[3,5-difluoro-6-(p-methoxybenzylamino)pyridin-2-yl]-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate, and the mixture was heated under reflux with stirring for 16 hours. The solution was allowed to cool and stand, and the precipitate was collected by decantation, and washed by adding a small amount of distilled water, shaking, allowing to stand, and decanting. To the precipitate was added 10 ml of ethanol, and the mixture was heated under reflux with stirring for 1 hour and allowed to cool and stand, and the precipitate was collected by decantation. To this precipitate was again added 10 ml of chloroform, and the mixture was stirred under reflux condition for 1 hour and allowed to cool, and the precipitate was collected by filtration and washed with ethanol and diisopropylether successively to obtain 1.25 g of the title compound as a pale brown powder.

1. temperaturethe mixture was heated
2. temperatureunder reflux
3. temperatureto cool
4. customthe precipitate was collected by decantation
5. washwashed
6. additionby adding a small amount of distilled water
7. stirringshaking
8. customdecanting
9. additionTo the precipitate was added 10 ml of ethanol
10. temperaturethe mixture was heated
11. temperatureunder reflux
12. stirringwith stirring for 1 hour
13. temperatureto cool
14. customthe precipitate was collected by decantation
15. stirringthe mixture was stirred
16. temperatureunder reflux condition for 1 hour
17. temperatureto cool
18. filtrationthe precipitate was collected by filtration
19. washwashed with ethanol and diisopropylether successively