反应详情

温度

120 °C

A solution of (3-amino-4-fluorophenoxy)acetic acid methyl ester (0.42 g) and 3-oxo-2-(4-pyrazol-1-ylbenzyl)pentanoic acid ethyl ester (0.63 g) in 1,4-dioxane (20 mL) was added to polyphosphoric acid (3 g) at 100° C., and the resulting mixture was stirred at 120° C. for 18 hours. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were washed with water and saturated aqueous sodium chloride solution, and then dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel, eluting with a mixture of cyclohexane and ethyl acetate to afford title compound (0.39 g).

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