反应详情

TBSOTf (360 μL, 1.57 mmol) was added to a 0° C. solution of 3-1 (235 mg, 1.04 mmol) and triethylamine (450 μL, 3.23 mmol) in dichloromethane (3 mL). The reaction was allowed to warm to room temperature and after 1 h, saturated NaHCO3 solution was added. The resulting mixture was extracted with ethyl acetate (3×30 mL) and the combined ethyl acetate solution was washed with brine. The solution was then dried (Na2SO4), filtered and evaporated. Purification by flash chromatography on silica gel (hexanes) gave 3-2 (329 mg, 93%).

1. extractionThe resulting mixture was extracted with ethyl acetate (3×30 mL)
2. washthe combined ethyl acetate solution was washed with brine
3. dry with materialThe solution was then dried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customPurification by flash chromatography on silica gel (hexanes)