HRID1757088

反应详情

EQUATION

反应方程式

HRID 1757088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 0.88 g of pyridinium dicromate in 2.20 ml of dichloromethane a solution of 0.50 g of 3β,14β-dihydroxy-5β-androstane-17β-carboxaldehyde (Boutagy J. and Thomas R., Aust. J. Chem., 1971, 24, 2723) in 2.5 ml of dichloromethane was added at room temperature. After 20 hrs the mixture was diluted with diethyl ether and filtered through celite; the filtrate was evaporated to dryness under reduced pressure. The crude product was purified by flash-chromatography (SiO2) using n-hexane/ethyl acetate 6/4 eluant; the fractions containing the title compound were collected and evaporated to give 0.30 g of the title compound (II-f) as a white foam.

WORKUP

后处理

  1. additionwas added at room temperature
  2. filtrationfiltered through celite
  3. customthe filtrate was evaporated to dryness under reduced pressure
  4. customThe crude product was purified by flash-chromatography (SiO2)
  5. additionthe fractions containing the title compound
  6. customwere collected
  7. customevaporated