반응 #92988

반응 방정식

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

sodium n-hexanoate

→

above-identified compound

수율 77.5%

16β-Ethyl-17β-n-hexanoyloxyacetoxy-4-estren-3-one

수율 77.5%

용매

acetone

반응 조건

후처리

1. 1
   온도the solution is refluxed for 6 hours
2. 2
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
3. 3
   추출the residue is extracted with 300 ml of ethyl acetate
4. 4
   기타The organic layer is separated
5. 5
   세척washed with water and saturated aqueous sodium chloride solution
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
8. 8
   세척passage of 750 ml of diisopropyl ether-n-hexane (9:1), elution
9. 9
   workup.ADDITIONis carried out with 1000 ml of a 1:1 mixture of the same solvents
10. 10
    기타The eluate is evaporated under reduced pressure
11. 11
    기타to remove the solvent

실험 절차

In 150 ml of 50% aqueous acetone are dissolved 5.0 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 2.5 g of sodium n-hexanoate and the solution is refluxed for 6 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 magnesium 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 (9:1), 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 4.2 g of the above-identified compound as a light-yellow viscous oil.

출처