HRID2377227
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
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
- temperatureThe mixture was cooled with an acetone/dry ice bath
- additionwas slowly added
- filtrationThe mixture was filtered
- customthe obtained solid was purified by flash chromatography on silica gel
- customThe product was further recrystallized from methanol