反应详情

A mixture of 1.28 g of ethyl 7-(1-t-butoxycarbonyl-3-pyrrolidinyloxy)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate, 3.5 ml of 1N aq. sodium hydroxide solution and 30 ml of tetrahydrofuran was heated under reflux for 1.5 hours. The mixture was concentrated under reduced pressure. To the residue was added 10% aq. citric acid to acidify the same, followed by extraction with chloroform. The chloroform layer was washed with saturated saline, dried over anhydrous sodium sulfate, and then concentrated to dryness. The residue was recrystallized from chloroform-diisopropyl ether, whereby 1.11 g of the title compound was obtained as colorless powder.

1. temperaturewas heated
2. temperatureunder reflux for 1.5 hours
3. concentrationThe mixture was concentrated under reduced pressure
4. additionTo the residue was added 10% aq. citric acid
5. extractionfollowed by extraction with chloroform
6. washThe chloroform layer was washed with saturated saline
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated to dryness
9. customThe residue was recrystallized from chloroform-diisopropyl ether