反应详情

712 mg of anhydrous potassium carbonate are introduced into a solution of 4.3 g of the alcohol prepared in Example (23d) in 47 ml of methanol and the mixture is stirred at room temperature for 3 hours. While cooling with ice, 0.72 ml of concentrated hydrochloric acid are then added dropwise to the reaction solution and the whole is concentrated in vacuo. The residue is dissolved in methylene chloride, the solution is dried over magnesium sulphate and concentrated in vacuo. The crude product is chromatographed over silica gel by gradient elution in methylene chloride/acetone. 2.85 g of the title compound are obtained.

1. additionare then added dropwise to the reaction solution
2. concentrationthe whole is concentrated in vacuo
3. dissolutionThe residue is dissolved in methylene chloride
4. dry with materialthe solution is dried over magnesium sulphate
5. concentrationconcentrated in vacuo
6. customThe crude product is chromatographed over silica gel by gradient elution in methylene chloride/acetone