HRID1182866
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
The title compound was obtained in 74% yield following the procedure described in Example 34 starting from (E)-3-[3-(R)-pyrrolidinyl]oxyimino-2α-fluoro-17β-hydroxyandrostan-6-one fumarate (Example 35, 73 mg) and hydroxylamine hydrochloride (11 mg). After evaporation of the solvent the crude reaction mixture was purified by flash chromatography (SiO2, CHCl3/MeOH/26% NH4OH 90/10/1). To the concentrated fractions, a stoichiometric amount of fumaric acid in MeOH was added. The resulting precipitate was rinsed with heptane and filtered to give the title compound I-bj.
WORKUP
后处理
- customAfter evaporation of the solvent the crude
- customreaction mixture
- customwas purified by flash chromatography (SiO2, CHCl3/MeOH/26% NH4OH 90/10/1)
- additionTo the concentrated fractions, a stoichiometric amount of fumaric acid in MeOH was added
- washThe resulting precipitate was rinsed with heptane
- filtrationfiltered