反应详情

To a solution of 2-(4-nitrophenoxy)ethanol (6.40 g) in DMF were added imidazole (4.75 g) and TBDMSCl (6.84 g) and reaction mixture was stirred at room temperature for 1 hr. The reaction was monitored on TLC using hexane:ethyl acetate (7:3) as mobile phase. After completion of the reaction, water was added and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent removed under reduced pressure. The crude material was purified by column chromatography eluted with 6% ethyl acetate in hexane to give, after concentration, 10 g of tert-butyldimethyl(2-(4-nitrophenoxy)ethoxy)silane.

1. additionwas added
2. extractionthe mixture was extracted with ethyl acetate
3. dry with materialThe organic layer was dried over sodium sulfate
4. customthe solvent removed under reduced pressure
5. customThe crude material was purified by column chromatography
6. washeluted with 6% ethyl acetate in hexane
7. customto give
8. concentrationafter concentration, 10 g of tert-butyldimethyl(2-(4-nitrophenoxy)ethoxy)silane