反应详情

To a solution of Example 180B (32 mg, 0.09 mmol) in acetonitrile (1 mL) was added iodotrimethylsilane (TMSI) (19 μL, 0.13 mmol). The reaction solution was stirred at room temperature for 3 h. After which, additional 1.5 equivalents of TMSI (19 μL) were added and stirring was continued for 2 h. The solution was quenched with water (2 mL) and extracted with ethyl acetate (2× 1 mL). The combined organic extracts were dried (Na2SO4) and concentrated in vacuo. Column chromatography on silica (70% ethyl acetate/hexane) afforded product as a white foam (24 mg, 77%). MS m/z 346.0 (M+H)+

1. stirringstirring
2. waitwas continued for 2 h
3. customThe solution was quenched with water (2 mL)
4. extractionextracted with ethyl acetate (2× 1 mL)
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. concentrationconcentrated in vacuo