HRID2359268

反应详情

EQUATION

反应方程式

HRID 2359268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-(3,4-dichlorobenzyl)benzoic acid (Preparation 148,150 mg, 0.54 mmol) in dichloromethane (25 mL) was added methanesulphonamide (153 mg, 1.61 mmol), 4-dimethylaminopyridine (196 mg, 1.61 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (307 mg, 1.61 mmol) and the mixture was stirred at room temperature for 5 hours. The mixture was diluted with dichloromethane, washed with water and 1M hydrochloric acid solution, dried over Na2SO4 and the solvent evaporated in vacuo. The crude product was purified by silica gel column chromatography eluting with 95:5 dichloromethane:methanol to afford the title compound (102 mg, 53%).

WORKUP

后处理

  1. washwashed with water and 1M hydrochloric acid solution
  2. dry with materialdried over Na2SO4
  3. customthe solvent evaporated in vacuo
  4. customThe crude product was purified by silica gel column chromatography
  5. washeluting with 95:5 dichloromethane