HRID840301

反应详情

EQUATION

反应方程式

HRID 840301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylate (10.0 g, 22 mmol) in dichloromethane (950 ml) was treated with boron trichloride dimethyl sulphide complex (40 ml, 2M, 80 mmol). The reaction was stirred at ambient temperature for 48 hours. Saturated aqueous sodium hydrogen carbonate solution was added and the layers were washed with dichloromethane. The organic layers were combined, dried (MgSO4) and evaporated to give an off white solid which was subjected to chromatography (eluant: ethyl acetate/hexane) to give methyl 2-[N-(5-bromo-2-hydroxybenzyl)-N-ethylamino]pyridine-5-carboxylate (6.02 g, 75%).

WORKUP

后处理

  1. washthe layers were washed with dichloromethane
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customto give an off white solid which