反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 200 ml of acetone-water (1:1) are added 6.0 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 5.2 g of sodium n-decanoate and the mixture is refluxed for 10 hours. The solvent is distilled off under reduced pressure and the residue is extracted with 300 ml of ethyl acetate. The organic layer is separated, 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 750 ml of diisopropyl ether-n-hexane (1:9), elution is carried out with 1000 ml of a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 5.2 g of the above-identified compound as a light-yellow viscous oil.
WORKUP
后处理
- temperaturethe mixture is refluxed for 10 hours
- distillationThe solvent is distilled off under reduced pressure
- extractionthe residue is extracted with 300 ml of ethyl acetate
- customThe organic layer is separated
- washwashed with water and saturated aqueous sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent is then distilled off under reduced pressure
- washpassage of 750 ml of diisopropyl ether-n-hexane (1:9), elution
- additionis carried out with 1000 ml of a 1:1 mixture of the same solvents
- customThe eluate is evaporated under reduced pressure
- customto remove the solvent