반응 #92990

반응 방정식

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

2-ethylbutyric acid

→

above-identified compound

16β-Ethyl-17β-(2-ethylbutyryl)oxyacetoxy-4-estren-3-one

용매

acetone

NaOH

반응 조건

후처리

1. 1
   온도The mixture is refluxed for 3 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
3. 3
   추출the residue is extracted with two 100 ml portions of ethyl acetate
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 50 ml of ether, elution
8. 8
   기타The eluate is evaporated under reduced pressure
9. 9
   기타to remove the solvent

실험 절차

In 35 ml of acetone is dissolved 1.0 ml of 2-ethylbutyric acid, and 4.6 ml of 2N-NaOH and then 1.9 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one are added to the above solution. The mixture is refluxed for 3 hours. The acetone is distilled off under reduced pressure and the residue is extracted with two 100 ml portions of ethyl acetate. The organic layers are combined, 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 50 ml of ether, elution is carried out with 300 ml of the same solvent. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.63 g of the above-identified compound as a light-yellow viscous oil.

출처