反应 #40269

反应方程式

4-(4-Aminophenyl)butyric acid

methanol

hydrogen chloride

→

methyl 4-(4-aminophenyl)butyrate hydrogen chloride

反应条件

后处理

1. 1
   其他was bubbled through the solution
2. 2
   温度After the reaction mixture was cooled to room temperature
3. 3
   workup.ADDITIONethyl ether (100 ml.) was added
4. 4
   其他The mixture, which separated into two layers
5. 5
   过滤The crystalline product was collected by filtration
6. 6
   其他dried thoroughly
7. 7
   其他The filtrate was evaporated to dryness
8. 8
   其他the residue was recrystallized from MeOH/benzene

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.

来源