反应详情

200 mg (0.625 mmol) of methyl 8-cyano-1-cyclopropyl-7-chloro-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate, 86 mg (0.683 mmol) of (1S,6S)-2,8-diazabicyclo[4.3.0]nonane and 150 mg (1.34 mmol) of 1,4-diazabicyclo[2.2.2]octane are stirred in 6 ml of acetonitrile at room temperature for 48 hours. Thereafter, the mixture is evaporated and the residue is partitioned between 15 ml of chloroform and 20 ml of saturated sodium carbonate solution. The organic phase is separated off, the aqueous phase is extracted again with chloroform and, after drying with sodium sulfate, the combined extracts are evaporated. For purification, the residue is chromatographed over silica gel with ethyl acetate/ethanol/25% strength aqueous ammonia solution.

1. customThereafter, the mixture is evaporated
2. customthe residue is partitioned between 15 ml of chloroform and 20 ml of saturated sodium carbonate solution
3. customThe organic phase is separated off
4. extractionthe aqueous phase is extracted again with chloroform
5. dry with materialafter drying with sodium sulfate
6. customthe combined extracts are evaporated
7. customFor purification
8. customthe residue is chromatographed over silica gel with ethyl acetate/ethanol/25% strength aqueous ammonia solution