反应详情

To a solution of 3 (15.7 g, 30.0 mmol) in methanol (100 mL) was added potassium carbonate (4.14 g, 30.0 mmol). After 1 h, saturated ammonium chloride (100 mL) and saturated brine (100 mL) were added, the mixture was extracted with methylene chloride (3×100 mL), dried (magnesium sulfate), filtered, concentrated, and chromatographed on a 15 cm tall×41 mm diameter silica gel column eluting with 40% ethyl acetate in hexane to afford 4 (9.93 g, 79%).

1. extractionthe mixture was extracted with methylene chloride (3×100 mL)
2. dry with materialdried (magnesium sulfate)
3. filtrationfiltered
4. concentrationconcentrated
5. customchromatographed on a 15 cm tall×41 mm diameter silica gel column
6. washeluting with 40% ethyl acetate in hexane