반응 #40269

반응 방정식

4-(4-Aminophenyl)butyric acid

methanol

hydrogen chloride

→

methyl 4-(4-aminophenyl)butyrate hydrogen chloride

반응 조건

후처리

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

실험 절차

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.

출처