反应详情

温度

70 °C

A mixture of [3-(4-chlorobenzyl)-8-fluoro-2-methyl-4-oxo-1,4-dihydroquinolin-5-yloxy]acetic acid methyl ester (0.29 g), N,N-dimethylformamide (10 mL), potassium carbonate (0.62 g) and acetic acid chlorodifluoromethyl ester (0.31 mL) was stirred at 70° C. for 17 hours. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were dried over sodium sulfate and the solvent removed under reduced pressure. Purification of the residue by column chromatography on silica gel, eluting with a mixture of cyclohexane and ethyl acetate (4:1 by volume) gave title compound, 0.18 g.

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. dry with materialThe combined extracts were dried over sodium sulfate
4. customthe solvent removed under reduced pressure
5. customPurification of the residue by column chromatography on silica gel
6. washeluting with a mixture of cyclohexane and ethyl acetate (4:1 by volume)