반응 #92987

반응 방정식

16β-ethyl-bromoacetoxy-4-estren-3-one

potassium isobutyrate

→

above-identified compound

수율 70.8%

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

수율 70.8%

용매

acetone

water

반응 조건

후처리

1. 1
   온도the solution is refluxed for 6 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
3. 3
   추출the residue is extracted with 200 ml of ethyl acetate
4. 4
   기타The organic layer is separated
5. 5
   세척washed with water and saturated aqueous sodium chloride
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
8. 8
   세척passage of 100 ml of diisopropyl ether, elution
9. 9
   기타The eluate is evaporated under reduced pressure
10. 10
    기타to remove the solvent

실험 절차

In a mixture of 50 ml of acetone and 10 ml of water are dissolved 1.5 g of 16β-ethyl-bromoacetoxy-4-estren-3-one and 0.8 g of potassium isobutyrate and the solution is refluxed for 6 hours. The acetone is distilled off under reduced pressure and the residue is extracted with 200 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride 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 100 ml of diisopropyl ether, elution is carried out with 300 ml of ethyl ether. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.08 g of the above-identified compound as a viscous oil.

출처