反应详情

温度

70 °C

A mixture of [8-fluoro-3-(4-fluorobenzyl)-4-methyl-2-oxo-1,2-dihydroquinolin-5-yloxy]acetic acid methyl ester (0.48 g), N,N-dimethylformamide (6.0 mL), potassium carbonate (0.72 g) and acetic acid chlorodifluoromethyl ester (1.7 mL) was stirred at 70° C. for 5 days. The mixture was diluted with Water, extracted with ethyl acetate and the combined extracts washed with water and then dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with a mixture of ethyl acetate and cyclohexane (1:6 by volume), followed by washing with diethyl ether gave title compound as a white solid, 0.29 g.

1. extractionextracted with ethyl acetate
2. washthe combined extracts washed with water
3. dry with materialdried over magnesium sulfate
4. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
5. washeluting with a mixture of ethyl acetate and cyclohexane (1:6 by volume)
6. washby washing with diethyl ether