反应详情

A mixture of 2.1 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 1.0 g of potassium acetate is stirred in a mixture of 50 ml of acetone and 3 ml of water for 20 hours. The acetone 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 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 700 ml of diisopropyl ether-n-hexane (1:1), elution is carried out with 600 ml of a 3:2 mixture and 300 ml of a 5:1 mixture of the same solvents. The eluates are combined and evaporated under reduced pressure to remove the solvent, giving 0.7 g of the above-identified compound as colorless crystals.

1. distillationThe acetone is distilled off under reduced pressure
2. extractionthe residue is extracted with 150 ml of ethyl acetate
3. customThe organic layer is separated
4. washwashed with water and saturated aqueous sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent is then distilled off under reduced pressure
7. washpassage of 700 ml of diisopropyl ether-n-hexane (1:1), elution
8. additionis carried out with 600 ml of a 3:2 mixture and 300 ml of a 5:1 mixture of the same solvents
9. customevaporated under reduced pressure
10. customto remove the solvent