反应详情

温度

80 °C

A mixture of [2-ethyl-8-fluoro-4-oxo-3-(4-pyrazol-1-ylbenzyl)-1,4-dihydroquinolin-5-yloxy]acetic acid methyl ester (0.37 g), N,N-dimethylformamide (10 mL), potassium carbonate (0.18 g) and acetic acid chlorodifluoromethyl ester (0.27 mL) was stirred at 80° C. for 6 hours. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated under reduced pressure. Purification of the residue by column chromatography on silica gel, eluting with a mixture of cyclohexane and ethyl acetate gave title compound (0.19 g).

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe combined extracts were washed with saturated aqueous sodium chloride solution
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customPurification of the residue by column chromatography on silica gel
7. washeluting with a mixture of cyclohexane and ethyl acetate