反应 #92989

反应方程式

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

4-methylvaleric acid

→

above-identified compound

16β-Ethyl-17β-(4-methylvaleryl)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 6 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure and 10 ml of water
3. 3
   workup.ADDITIONis added to the residue
4. 4
   萃取followed by extraction with 100 ml of ethyl acetate
5. 5
   其他The organic layer is separated
6. 6
   洗涤washed with water and saturated aqueous sodium chloride solution
7. 7
   干燥dried over anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONThe solvent is then distilled off
9. 9
   洗涤the residue is subjected to column chromatography, elution
10. 10
    其他The eluate is evaporated under reduced pressure
11. 11
    其他to remove the solvent

实验过程

In 35 ml of acetone is dissolved 1.0 ml of 4-methylvaleric 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 6 hours. The acetone is distilled off under reduced pressure and 10 ml of water is added to the residue, followed by extraction with 100 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent is then distilled off and the residue is subjected to column chromatography, elution being carried out with 600 ml of diisopropyl ether-n-hexane (1:1). The eluate is evaporated under reduced pressure to remove the solvent, giving 1.3 g of the above-identified compound as a colorless viscous oil.

来源