反应详情

A mixture of 2-(2-bromothiophen-3-yl)ethanol (4.5 g, 21.8 mmol), tert-butylchloro-dimethylsilane (3.16 g, 24.0 mmol) and imidazole (1.63 g, 24.0 mmol) in N,N-dimethylformamide (40 mL) was stirred at rt for 24 h. 100 mL of water was added and the mixture was extracted with diethyl ether (3×00 mL). The combined organic layers were washed with brine (3×100 mL), dried over anhydrous sodium sulfate and filtered. The solvent was removed in vacuo and the product purified by flash chromatography eluting with ethyl acetate/hexane (1:20) to give the title compound as an oil (5.9 g, 84%).

1. extractionthe mixture was extracted with diethyl ether (3×00 mL)
2. washThe combined organic layers were washed with brine (3×100 mL)
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. customThe solvent was removed in vacuo
6. customthe product purified by flash chromatography
7. washeluting with ethyl acetate/hexane (1:20)