反应详情

After dissolving 3,4-dibromo-6-ethoxy-2-fluorophenol (3.8 g, 12 mmol) in dimethylformamide (30 ml), methyl iodide (1.5 ml, 24 mmol) and potassium carbonate (3.3 g, 24 mmol) were added and the mixture was stirred at room temperature for 18 hours. Water (80 ml) was added, extraction was performed with diethyl ether (60 ml×2), and then after washing the combined organic layers with brine (80 ml) and drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (1.83 g, 46.7%).

1. additionwere added
2. extractionextraction
3. washafter washing the combined organic layers with brine (80 ml)
4. dry with materialdrying over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)