HRID2377227

反应详情

EQUATION

反应方程式

HRID 2377227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 2-(2-carboxyethyl)benzoic acid (1.0 g, 5.15 mmol), sodium chloride (320 mg, 5.41 mmol) and aluminum chloride (3.43 g, 25.75 mmol) was heated to about 160° C. for about 2 hours. The mixture was cooled with an acetone/dry ice bath and a mixture of ice and water was slowly added, followed by concentrated hydrochloric acid (AMOUNT). The mixture was filtered and the obtained solid was purified by flash chromatography on silica gel using dichloromethane/methanol (50:1) as eluent. The product was further recrystallized from methanol to provide the desired product. MS (ESI): m/z 175 (M−H)−.

WORKUP

后处理

  1. temperatureThe mixture was cooled with an acetone/dry ice bath
  2. additionwas slowly added
  3. filtrationThe mixture was filtered
  4. customthe obtained solid was purified by flash chromatography on silica gel
  5. customThe product was further recrystallized from methanol