反应详情

In 30 ml of acetone is dissolved 0.49 g of benzoic acid, and 2 ml of 2 N-NaOH and 5 ml of water are added, followed by addition of 0.88 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one. The mixture is refluxed for 3 hours. After cooling, the solvent is distilled off under reduced pressure and the residue is extracted with 100 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 chromatographed on a silica gel column. After passage of 350 ml of diisopropyl ether, the solvent is distilled off under reduced pressure. To the residue is added a small amount of diisopropyl ether, followed by filtration to give 0.86 g of the above-identified compound as a white powder.

1. additionare added
2. temperatureThe mixture is refluxed for 3 hours
3. temperatureAfter cooling
4. distillationthe solvent is distilled off under reduced pressure
5. extractionthe residue is extracted with 100 ml of ethyl acetate
6. customThe organic layer is separated
7. washwashed with water and saturated aqueous sodium chloride solution
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationThe solvent is then distilled off under reduced pressure
10. customthe residue is chromatographed on a silica gel column
11. distillationAfter passage of 350 ml of diisopropyl ether, the solvent is distilled off under reduced pressure
12. additionTo the residue is added a small amount of diisopropyl ether
13. filtrationfollowed by filtration