HRID440541

反应详情

EQUATION

反应方程式

HRID 440541 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of tetrakis triphenylphosphine palladium (7 g), 3-bromo-4-methoxyphenethylamine hydrobromide (62.2 g) and toluene (400 ml) was stirred under nitrogen with 2M aqueous sodium carbonate solution (200 ml) and then a solution of phenyl boric acid (26.8 g) in ethanol (100 ml) was added. The mixture was heated under reflux for 48 hours then cooled and treated with 30% aqueous hydrogen peroxide solution (10 ml). The mixture was stirred at ambient temperature for 1 hour. The aqueous layer was separated and extracted with ether. The ether extracts were combined with the original organic phase. Distillation yielded 4-methoxy-3-phenylphenethylamine which was used without further purification.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 48 hours
  3. temperaturethen cooled
  4. customThe aqueous layer was separated
  5. extractionextracted with ether
  6. distillationDistillation