反応 #92994

反応方程式

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

sodium stearate

→

above-identified compound

収率 57.1%

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

収率 57.1%

溶媒

acetone water

反応条件

後処理

1. 1
   温度the mixture is refluxed for 4 hours
2. 2
   その他to stand at room temperature
3. 3
   その他(15°-25° C.) overnight
4. 4
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
5. 5
   抽出the residue is extracted with 150 ml of ethyl acetate
6. 6
   その他The organic layer is separated
7. 7
   洗浄washed with water and saturated aqueous sodium chloride
8. 8
   乾燥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
    ろ過the insoluble material is filtered off
13. 13
    workup.DISTILLATIONThe solvent is distilled off
14. 14
    その他to give a colorless viscous oil, which
15. 15
    その他to stand at room temperature
16. 16
    その他(15°-25° C.)

実験手順

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.

出典