反应详情

温度

0 °C

Chlorotriisopropylsilane (0.640 g, 0.71 mL, 3.3 mmol) was added dropwise to a 0° C. cooled solution of 13 (0.450 g, 3.0 mmol) and 1H-imidazole (0.410 g, 6.0 mmol) in anhydrous N,N-dimethylformamide (10 mL). The reaction mixture was stirred at 0° C. for 3 h and then diluted with water. The resulting mixture was extracted with diethyl ether, and the combined organic layers were washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue was purified by silica gel column chromatography using ethyl acetate-hexanes 1:9 as eluent to furnish the desired compound as colorless oil. Yield: 96%.

1. extractionThe resulting mixture was extracted with diethyl ether
2. washthe combined organic layers were washed with brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by silica gel column chromatography