反应详情

The compound of Example 13B (16.0 g, 42 mmol) was dissolved in 20 mL of dimethylformamide; 7.1 g of imidazole (100 mmol, 2.5 equivalents) was added, followed by 10.5 mL of chlorotriethylsilane. The resultant mixture was stirred overnight at ambient temperature, then was diluted with water and extracted with ethyl acetate. The organic phase was concentrated washed with brine and dried over Na2SO4. After concentrating in vacuo, the residue was purified by flash chromatography, eluting with a gradient from 50% to 100% dichloromethane in hexanes to provide the titled compound (14.0 g, 90%).

1. extractionextracted with ethyl acetate
2. concentrationThe organic phase was concentrated
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. concentrationAfter concentrating in vacuo
6. customthe residue was purified by flash chromatography
7. washeluting with a gradient from 50% to 100% dichloromethane in hexanes