HRID1182866

反应详情

EQUATION

反应方程式

HRID 1182866 的结构方程式

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

  1. customAfter evaporation of the solvent the crude
  2. customreaction mixture
  3. customwas purified by flash chromatography (SiO2, CHCl3/MeOH/26% NH4OH 90/10/1)
  4. additionTo the concentrated fractions, a stoichiometric amount of fumaric acid in MeOH was added
  5. washThe resulting precipitate was rinsed with heptane
  6. filtrationfiltered