反应详情

A solution of 5-fluoro-6-hydroxy-7-iodobenzofuran-3(2H)-one (0.256 g, 0.871 mmol) in DMF (5 mL) was added with potassium carbonate (0.110 g, 0.796 mmol). The mixture was added with dimethyl sulfate (0.0803 g, 0.637 mmol) at room temperature, and the mixture was stirred for 12 hours. The reaction mixture was added with water, the mixture was extracted with ethyl acetate, and the organic layer was washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate, then the solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain 5-fluoro-7-iodo-6-methoxybenzofuran-3(2H)-one (0.0582 g, 21%).

1. extractionthe mixture was extracted with ethyl acetate
2. washthe organic layer was washed with saturated brine
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. customthe solvent was evaporated
5. customthe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate)