HRID11991

反应详情

EQUATION

反应方程式

HRID 11991 的结构方程式

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

4-(4-Aminophenyl)butyric acid (5 g) was dissolved in 40 ml methanol. The solution was refluxed at 80-90° C. with stirring for 4 h while hydrogen chloride gas was bubbled through the solution. After the reaction mixture was cooled to room temperature, ethyl ether (100 ml.) was added. The mixture, which separated into two layers, was refrigerated overnight. The crystalline product was collected by filtration and dried thoroughly. The filtrate was evaporated to dryness and the residue was recrystallized from MeOH/benzene. The total amount of the product methyl 4-(4-aminophenyl)butyrate hydrogen chloride obtained was 5.6 g (87.5%), m.p. 143-145° C.

WORKUP

后处理

  1. customwas bubbled through the solution
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. additionethyl ether (100 ml.) was added
  4. customThe mixture, which separated into two layers
  5. filtrationThe crystalline product was collected by filtration
  6. customdried thoroughly
  7. customThe filtrate was evaporated to dryness
  8. customthe residue was recrystallized from MeOH/benzene