反应详情

To a solution of 2 (2.40 g, 8.8 mmol), 4-(dimethylamino)pyridine (100 mg, 0.82 mmol), and imidazole (1.00 g, 14.7 mmol) in methylene chloride (35 mL) was added dropwise t-butyldiphenylchlorosilane (2.85 g, 10.4 mmol). After stirring overnight, the mixture was added to saturated ammonium chloride (40 mL), extracted with ethyl acetate (3×40 mL), dried (magnesium sulfate), filtered, concentrated, and chromatographed on a 14 cm tall×53 mm diameter silica gel eluting with 30% ethyl acetate in hexane to afford 3 (3.776 g, 83%).

1. extractionextracted with ethyl acetate (3×40 mL)
2. dry with materialdried (magnesium sulfate)
3. filtrationfiltered
4. concentrationconcentrated
5. customchromatographed on a 14 cm tall×53 mm