反应详情

In 20 ml of acetonitrile were dissolved 344 mg of 8-chloro-6,7-difluoro-1-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 490 mg of (S,S)-1-t-butoxycarbonyloctahydropyrrolo[3.4-b]pyridine (also termed "(S,S)-2-t-butoxycarbonyl-2,8-azabicyclo[4.3.0]nonane"), and 1 ml of triethylamine, and the solution was heated under reflux for 5 hours. After completion of the reaction, the solvent was removed under reduced pressure. To a residue was added 30 ml of water, followed by extracting with chloroform (30 ml×4). The combined organic layer was washed with 100 ml of a 10% citric acid aqueous solution and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and a residue was recrystallized from acetonitrile to yield 317 mg of the titled compound.

1. temperaturethe solution was heated
2. temperatureunder reflux for 5 hours
3. customAfter completion of the reaction
4. customthe solvent was removed under reduced pressure
5. additionTo a residue was added 30 ml of water
6. extractionby extracting with chloroform (30 ml×4)
7. washThe combined organic layer was washed with 100 ml of a 10% citric acid aqueous solution
8. dry with materialdried over anhydrous sodium sulfate
9. customThe solvent was removed under reduced pressure
10. customa residue was recrystallized from acetonitrile