反应详情

In 40 ml of DMF is dissolved 0.6 g of α-hydroxybutyric acid, and 6.0 ml of 1N-NaOH and 1.4 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one are added. The mixture is stirred at room temperature (15°-25° C.) for 16 hours. To the reaction mixture is added 150 ml of ethyl acetate and the mixture is washed with water and saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 50 ml of dichloromethane and 100 ml of diisopropyl ether in that order, elution is carried out with 150 ml of diisopropyl ether and 250 ml of diisopropyl ether-ethyl acetate (1:10). The eluates are combined and evaporated under reduced pressure to remove the solvent, giving 0.82 g of the above-identified compound as a colorless viscous oil.

1. additionare added
2. washthe mixture is washed with water and saturated aqueous sodium chloride solution
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent is then distilled off under reduced pressure
5. washin that order, elution
6. customevaporated under reduced pressure
7. customto remove the solvent