HRID1757088
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added at room temperature
- filtrationfiltered through celite
- customthe filtrate was evaporated to dryness under reduced pressure
- customThe crude product was purified by flash-chromatography (SiO2)
- additionthe fractions containing the title compound
- customwere collected
- customevaporated