反应详情

温度

50 °C

To a solution of 6.73 g (43.7 mmol) of 3,5-dimethoxyphenol in anhydrous dimethylformamide (50 mL) were added 5.95 g (87.4 mmol) of imidazole and 15.0 g (54.6 mmol) of t-butylchlorodiphenylsilane. The mixture was stirred at 50° C. for 4 hours. Water was added and the mixture was extracted with ethyl acetate-hexane (1:2). The organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, whereby 16.14 g of 1-t-butyldiphenylsiloxy-3,5-dimethoxybenzene was obtained as a colorless crystalline powder (mp: 95.5 to 96.5° C., yield: 94%).

1. extractionthe mixture was extracted with ethyl acetate-hexane (1:2)
2. washThe organic layer was washed with water
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography on silica gel