HRID1455950
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
To a solution of 2-(N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylic acid (0.89 g) in dichloromethane (50 ml) was added propanesulphonamide (0.3 g), dimethylaminopyrimidine (0.493 g) and 1-(3-dimethylaminopropyl)ethylcarbodiimide hydrochloride (0.58 g). The mixture was stirred at ambient temperature for 18 hours, and poured into 2N HCl. The organic layer was separated and washed with water and brine, then dried (MgSO4), filtered and evaporated. The resulting oil was purified by chromatography on silica gel (eluting with 5% ethylacetate/dichloromethane to give N-(2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carbonyl)propanesulphonamide (271 mg) as a white foam.
WORKUP
后处理
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe resulting oil was purified by chromatography on silica gel (
- washeluting with 5% ethylacetate/dichloromethane