反応 #92991

反応方程式

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

n-octanoic acid

→

above-identified compound

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

溶媒

acetone

NaOH

water

反応条件

後処理

1. 1
   workup.ADDITIONare serially added to the above solution
2. 2
   温度The mixture is refluxed for 4 hours
3. 3
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
4. 4
   抽出the residue is extracted with 150 ml of ethyl acetate
5. 5
   その他The organic layer is separated
6. 6
   洗浄washed with water and saturated aqueous sodium chloride solution
7. 7
   乾燥dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
9. 9
   洗浄passage of 50 ml of diisopropyl ether, elution
10. 10
    その他The eluate is evaporated under reduced pressure
11. 11
    その他to remove the solvent

実験手順

In 60 ml of acetone is dissolved 1.0 ml of n-octanoic acid, and 3.0 ml of 2N-NaOH, 15 ml of water and 1.8 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one are serially added to the above solution. The mixture is refluxed for 4 hours. The solvent 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 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 50 ml of diisopropyl ether, elution is carried out with 300 ml of the same solvent. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.7 g of the above-identified compound as a colorless oil.

出典