HRID2414820

反应详情

EQUATION

反应方程式

HRID 2414820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred suspension of LAH (8.0 g, 0.21 mol) in THF (300 mL) is cooled in an ice bath and a solution of 4-benzyloxy-3-methoxynitrostyrene (15.0 g, 52.6 mmol) in THF (300 mL) is added dropwise. The green reaction mixture is allowed to warm to room temperature over 0.5 h, and is then refluxed for 4 h. The grey reaction mixture is treated successively with water (8 mL), 15% aqueous NaOH (8 mL), and water (24 mL). The resulting gray suspension is stirred at 50° C. for 20 min. The resulting yellow suspension is filtered, and the residue is washed with EtOAc. The combined filtrates are evaporated to provide the title compound as yellow oil which is used without further purification.

WORKUP

后处理

  1. temperatureis cooled in an ice bath
  2. temperatureis then refluxed for 4 h
  3. filtrationThe resulting yellow suspension is filtered
  4. washthe residue is washed with EtOAc
  5. customThe combined filtrates are evaporated