반응 #92985

반응 방정식

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

potassium acetate

→

above-identified compound

수율 35.1%

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

수율 35.1%

용매

acetone

water

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
2. 2
   추출the residue is extracted with 150 ml of ethyl acetate
3. 3
   기타The organic layer is separated
4. 4
   세척washed with water and saturated aqueous sodium chloride
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
7. 7
   세척passage of 700 ml of diisopropyl ether-n-hexane (1:1), elution
8. 8
   workup.ADDITIONis carried out with 600 ml of a 3:2 mixture and 300 ml of a 5:1 mixture of the same solvents
9. 9
   기타evaporated under reduced pressure
10. 10
    기타to remove the solvent

실험 절차

A mixture of 2.1 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 1.0 g of potassium acetate is stirred in a mixture of 50 ml of acetone and 3 ml of water for 20 hours. The acetone is 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 magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 700 ml of diisopropyl ether-n-hexane (1:1), elution is carried out with 600 ml of a 3:2 mixture and 300 ml of a 5:1 mixture of the same solvents. The eluates are combined and evaporated under reduced pressure to remove the solvent, giving 0.7 g of the above-identified compound as colorless crystals.

출처