反应详情

A mixture of 4-nitrobenzylalcohol(10.0 g), tertbutyl-dimethylsilyl chloride (11.8 g), imidazole (11.2 g) and DMF (50 ml) was stirred at room temperature for 1.5 hours. To the mixture was added water (500 ml), and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/hexane=1/7) to give tert-butyldimethyl-4-nitrobenzyloxysilane (17.5 g) as pale yellow oil.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with saturated sodium chloride solution
3. dry with materialdried with anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was separated
6. custompurified with column chromatography (ethyl acetate/hexane=1/7)