反应详情

In 60 ml of acetone is dissolved 1.0 ml of n-octanoic acid, and 3.0 ml of 2N-NaOH, 15 ml of water and 1.8 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one are serially added to the above solution. The mixture is refluxed for 4 hours. The solvent is distilled off under reduced pressure and the residue is extracted with 150 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 50 ml of diisopropyl ether, elution is carried out with 300 ml of the same solvent. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.7 g of the above-identified compound as a colorless oil.

1. additionare serially added to the above solution
2. temperatureThe mixture is refluxed for 4 hours
3. distillationThe solvent is distilled off under reduced pressure
4. extractionthe residue is extracted with 150 ml of ethyl acetate
5. customThe organic layer is separated
6. washwashed with water and saturated aqueous sodium chloride solution
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationThe solvent is then distilled off under reduced pressure
9. washpassage of 50 ml of diisopropyl ether, elution
10. customThe eluate is evaporated under reduced pressure
11. customto remove the solvent