反应详情

温度

160 °C

To a solution of 2-bromo-4-fluoro-benzoic acid methyl ester (488 mg, 2.09 mmol) in anhydrous DMF (15 ml), 4-ethylphenol (256 mg, 2.09 mmol) and potassium carbonate (289 mg, 2.09 mmol) were added at room temperature, followed by stirring under a nitrogen atmosphere for 16 hours at 160° C. The reaction mixture was cooled and, after addition of saturated aqueous ammonium chloride, was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride and dried over sodium sulfate. After filtration, the solvent was distilled off under reduced pressure and the resulting residue was purified by silica gel column chromatography (developing solution=ethyl acetate:n-hexane (1:20)) to give the titled compound (455 mg, 65%).

1. temperatureThe reaction mixture was cooled
2. extractionwas then extracted with ethyl acetate
3. washThe organic layer was washed with saturated aqueous sodium chloride
4. dry with materialdried over sodium sulfate
5. filtrationAfter filtration
6. distillationthe solvent was distilled off under reduced pressure
7. customthe resulting residue was purified by silica gel column chromatography (developing solution=ethyl acetate:n-hexane (1:20))