反応 #40269

反応方程式

4-(4-Aminophenyl)butyric acid

methanol

hydrogen chloride

→

methyl 4-(4-aminophenyl)butyrate hydrogen chloride

反応条件

後処理

1. 1
   その他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
   その他The mixture, which separated into two layers
5. 5
   ろ過The crystalline product was collected by filtration
6. 6
   その他dried thoroughly
7. 7
   その他The filtrate was evaporated to dryness
8. 8
   その他the residue was recrystallized from MeOH/benzene

実験手順

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.

出典