HRID840301
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- washthe layers were washed with dichloromethane
- dry with materialdried (MgSO4)
- customevaporated
- customto give an off white solid which