反应详情

A mixture of ethyl 2-ethoxy-4′-fluoro-6-(((trifluoromethyl)sulfonyl)oxy)biphenyl-4-carboxylate (15.6 g), cyclopropylboronic acid (7.67 g), dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (2.20 g), a 2 M aqueous sodium carbonate solution (53.6 mL), tris(dibenzylideneacetone)dipalladium(0) (2.29 g), and toluene (60 mL) was stirred at 100° C. for 2 hours in an argon atmosphere. The reaction mixture was allowed to cool to room temperature and then poured to water, followed by extraction with ethyl acetate. The obtained organic layer was washed with saturated saline and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (10.5 g).

1. extractionfollowed by extraction with ethyl acetate
2. washThe obtained organic layer was washed with saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)