反応 #92990

反応方程式

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

2-ethylbutyric acid

→

above-identified compound

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

溶媒

acetone

NaOH

反応条件

後処理

1. 1
   温度The mixture is refluxed for 3 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
3. 3
   抽出the residue is extracted with two 100 ml portions of ethyl acetate
4. 4
   洗浄washed with water and saturated aqueous sodium chloride
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
7. 7
   洗浄passage of 50 ml of ether, elution
8. 8
   その他The eluate is evaporated under reduced pressure
9. 9
   その他to remove the solvent

実験手順

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.

出典