反应详情

To a mixed solution of 2.5 ml of 4N hydrochloric acid and 2.5 ml of acetic acid was added all amount of the above described ethyl 8-chloro-1-[3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine-2-yl]-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate, and the mixture was heated under reflux with stirring for 3 hours and allowed to cool and stand. To the residue was added 10 ml of distilled water, and the solution was concentrated under reduced pressure. The procedure of adding 10 ml of ethanol and concentrating the solution under reduced pressure was repeated three times, and 6 ml of chloroform was added to the residue, and the mixture was heated under reflux with stirring for 1 hour and allowed to cool. The precipitate was collected by filtration, and washed with ethanol and diisopropylether successively to obtain 128 mg of the title compound as a colorless powder.

1. temperaturethe mixture was heated
2. temperatureunder reflux
3. temperatureto cool
4. concentrationthe solution was concentrated under reduced pressure
5. additionThe procedure of adding 10 ml of ethanol
6. concentrationconcentrating the solution under reduced pressure
7. additionwas added to the residue
8. temperaturethe mixture was heated
9. temperatureunder reflux
10. stirringwith stirring for 1 hour
11. temperatureto cool
12. filtrationThe precipitate was collected by filtration
13. washwashed with ethanol and diisopropylether successively