HRID527016

反应详情

EQUATION

反应方程式

HRID 527016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of racemic [1-Hydroxy-3-methoxy-2-cyclohexanoxy]tert-butyl-dimethylsilane, 51f, (2.5 g; 9.6 mmol) in 60 mL of dry THF at room temperature was added, triphenylphosphine (5.0 g; 19.2 mmol), DIAD (3.9 g; 19.2 mmol) and diphenylphosphoryl azide (5.3 g; 19.2 mmol) and the reaction mixture was stirred at room temperature for 60 h. The solvent was concentrated in vacuo and the resultant oil was purified by silica gel chromatography (10% Et2O-Hexane to ether gradient) to afford 2.57 g of the desired product 51 g.

WORKUP

后处理

  1. concentrationThe solvent was concentrated in vacuo
  2. customthe resultant oil was purified by silica gel chromatography (10% Et2O-Hexane to ether gradient)