反应详情

温度

100 °C

After a 2M aqueous sodium carbonate solution (1.5 ml), tris(dibenzylideneacetone)dipalladium (0) (23 mg, 25 μmol) and bis(2-diphenylphosphinophenyl)ether (DPEphos) (28 mg, 52 μmol) were added to a solution of methyl (3-chloro-4-{[(trifluoromethyl)sulfonyl]oxy}phenyl)acetate (317 mg, 1.0 mmol) obtained in Example (23-1) and 4-methoxyphenylboronic acid (152 mg, 1.0 mmol) in a mixture of toluene-ethanol (5:1, 9 ml), the mixture was stirred at 100° C. for 5 hours under stirring. After the temperature of the reaction mixture was returned to room temperature, the mixture was poured into water and extracted with ethyl acetate (three times). The organic layer was successively washed with water (twice) and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. The solvent was removed under reduced pressure to give methyl (2-chloro-4′-methoxy-1,1′-biphenyl-4-yl)acetate as a solid (192 mg, yield: 66%).

1. stirringunder stirring
2. customwas returned to room temperature
3. extractionextracted with ethyl acetate (three times)
4. washThe organic layer was successively washed with water (twice) and a saturated aqueous NaCl solution
5. dry with materialdried with anhydrous sodium sulfate
6. customThe solvent was removed under reduced pressure