HRID230614

反应详情

EQUATION

反应方程式

HRID 230614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-bromophenylacetic acid (960 mg, 4.49 mmol) in dichloromethane (30 ml) was treated in one portion with solid 1,1′-carbonyldiimidazole (730 mg, 4.5 mmol) at 20° C. with stirring under argon. This mixture was allowed to stir at room temperature for 15 minutes. Triethylamine (0.63 ml) was then added followed by dimethylamine hydrochloride (367 mg, 4.5 mmol) and the stirring continued for 1 hour. Most of the solvent was removed under reduced pressure and the residue added to a 20 g isolute silica sep-pak column and eluted from 0-50% ethyl acetate in petroleum ether to give the title compound as a colourless solid (689 mg, 64%).

WORKUP

后处理

  1. stirringto stir at room temperature for 15 minutes
  2. customMost of the solvent was removed under reduced pressure
  3. additionthe residue added to a 20 g isolute silica sep-pak column
  4. washeluted from 0-50% ethyl acetate in petroleum ether