반응 #92986

반응 방정식

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

potassium propionate

→

above-identified compound

수율 35.4%

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

수율 35.4%

용매

acetone

water

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   추출The residue is extracted with 200 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 distilled off under reduced pressure
7. 7
   세척passage of 1000 ml isopropyl ether-n-hexane (2:3), elution
8. 8
   기타The eluate is evaporated under reduced pressure
9. 9
   기타to remove the solvent

실험 절차

In a mixture of 50 ml of acetone and 12 ml of water are dissolved 2.5 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 0.7 g of potassium propionate. The solution is stirred at room temperature (17°-25° C.) for 3 days and concentrated under reduced pressure. 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 distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 1000 ml isopropyl ether-n-hexane (2:3), elution is carried out with 2000 ml of the same solvent system. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.87 g of the above-identified compound as white crystals.

출처