HRID380051

反应详情

EQUATION

反应方程式

HRID 380051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Prepared according to the method described in Example 1d) from (3RS,4S)-4-(4-bromophenoxy)-1-pyridin-3-yl-hex-1-yn-3-ol (3.42 g, Example 87c)) and 5% rhodium on carbon (0.5 g) in ethyl acetate (100 ml). After work up crude material was purified by flash column chromatography over silica eluting with ethyl acetate to give a mixture of diastereomers. The mixture was separated by normal-phase HPLC eluting with 2% propan-2-ol in dichloromethane to give the sub-title compound as the second eluting, major diastereomer (2 g).

WORKUP

后处理

  1. customPrepared
  2. customAfter work up crude material was purified by flash column chromatography over silica eluting with ethyl acetate
  3. customto give
  4. additiona mixture of diastereomers
  5. customThe mixture was separated by normal-phase
  6. washHPLC eluting with 2% propan-2-ol in dichloromethane