반응 #92994

반응 방정식

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

sodium stearate

→

above-identified compound

수율 57.1%

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

수율 57.1%

용매

acetone water

반응 조건

후처리

1. 1
   온도the mixture is refluxed for 4 hours
2. 2
   기타to stand at room temperature
3. 3
   기타(15°-25° C.) overnight
4. 4
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
5. 5
   추출the residue is extracted with 150 ml of ethyl acetate
6. 6
   기타The organic layer is separated
7. 7
   세척washed with water and saturated aqueous sodium chloride
8. 8
   건조dried 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
    여과the insoluble material is filtered off
13. 13
    workup.DISTILLATIONThe solvent is distilled off
14. 14
    기타to give a colorless viscous oil, which
15. 15
    기타to stand at room temperature
16. 16
    기타(15°-25° C.)

실험 절차

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.

출처