反应 #92994

反应方程式

16β-ethyl-17β-bromoacetoxy-4-estren-3-one

sodium stearate

→

above-identified compound

收率 57.1%

16β-Ethyl-17β-stearoyloxyacetoxy-4-estren-3-one

收率 57.1%

溶剂

acetone water

反应条件

后处理

1. 1
   温度the mixture is refluxed for 4 hours
2. 2
   其他to stand at room temperature
3. 3
   其他(15°-25° C.) overnight
4. 4
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
5. 5
   萃取the residue is extracted with 150 ml of ethyl acetate
6. 6
   其他The organic layer is separated
7. 7
   洗涤washed with water and saturated aqueous sodium chloride
8. 8
   干燥dried over anhydrous sodium sulfate
9. 9
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
10. 10
    workup.DISSOLUTIONthe residue is dissolved in 100 ml of ethanol
11. 11
    workup.ADDITIONTo the solution is added 0.3 g of activated carbon
12. 12
    过滤the insoluble material is filtered off
13. 13
    workup.DISTILLATIONThe solvent is distilled off
14. 14
    其他to give a colorless viscous oil, which
15. 15
    其他to stand at room temperature
16. 16
    其他(15°-25° C.)

实验过程

To 150 ml of acetone-water (2:1) are added 1.3 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 1.0 g of sodium stearate and the mixture is refluxed for 4 hours and allowed to stand at room temperature (15°-25° C.) overnight. The solvent is then 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 sodium sulfate. The solvent is distilled off under reduced pressure and the residue is dissolved in 100 ml of ethanol. To the solution is added 0.3 g of activated carbon and the insoluble material is filtered off. The solvent is distilled off to give a colorless viscous oil, which is allowed to stand at room temperature (15°-25° C.) to give 1.1 g of the above-identified compound as a solid.

来源