HRID64735

反应详情

EQUATION

反应方程式

HRID 64735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a mixture of 2 ml of water and 2 ml of acetone is dissolved 0.26 g of sodium isovalerate, and 0.45 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 10 ml of DMF are added to the above solution. The mixture is refluxed for 6 hours, and thereafter treated in the same manner as Example 26. The reaction mixture is then subjected to column chromatography. Following passage of 100 ml of diisopropyl ether-n-hexane (2:8), elution is carried out with 400 ml of a 1:1 mixture of the same solvents. The elutate is evaporated under reduced pressure to remove the solvent, giving 0.415 g of the above-identified compound as a colorless viscous oil.

WORKUP

后处理

  1. additionare added to the above solution
  2. temperatureThe mixture is refluxed for 6 hours
  3. additiontreated in the same manner as Example 26
  4. washpassage of 100 ml of diisopropyl ether-n-hexane (2:8), elution
  5. additionis carried out with 400 ml of a 1:1 mixture of the same solvents
  6. customThe elutate is evaporated under reduced pressure
  7. customto remove the solvent