反应 #92990

反应方程式

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

2-ethylbutyric acid

→

above-identified compound

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

溶剂

acetone

NaOH

反应条件

后处理

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

实验过程

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.

来源