反应详情

Dibromoisocyanuric acid (15.9 g) was added at room temperature to a DMF (150 mL) solution of methyl 3-(benzyloxy)-2′,4′-difluorobiphenyl-4-carboxylate (28.0 g), and the mixture was stirred overnight at room temperature. Water was added to the reaction mixture at room temperature, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and saturated saline in this order 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 (34.0 g)

1. extractionfollowed by extraction with ethyl acetate
2. washThe obtained organic layer was washed with water and saturated saline in this order
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)