반응 #326894

반응 방정식

4-(4-fluorophenyl)-1,2,3,6-tetrahydropyridine

1,3-propane sultone

→

3-[4-(4-fluorophenyl)-1,2,3,6-tetrahydropyridin-1-yl]-1-propanesulfonic acid

용매

acetone

반응 조건

후처리

1. 1
   온도at reflux overnight
2. 2
   기타Only a small amount of compound precipitated
3. 3
   기타a larger amount of solid precipitated
4. 4
   온도The suspension was heated with the addition of a small amount of MeOH until complete dissolution of the solid
5. 5
   workup.STIRRINGThe resulting solution was stirred
6. 6
   온도at reflux for a few minutes
7. 7
   온도was cooled to room temperature with stiffing
8. 8
   여과The solid was collected by filtration
9. 9
   세척washed with MeOH
10. 10
    기타dried in vacuo

실험 절차

To a solution of 4-(4-fluorophenyl)-1,2,3,6-tetrahydropyridine (1.96 g, 13.7 mmol) in acetone (30 mL) was added 1,3-propane sultone (1.74 g, 14.5 mmol). The mixture was stirred at reflux overnight. Only a small amount of compound precipitated. The resulting suspension was cooled to room temperature with stiffing and a larger amount of solid precipitated. The suspension was heated with the addition of a small amount of MeOH until complete dissolution of the solid. The resulting solution was stirred at reflux for a few minutes and was cooled to room temperature with stiffing. The solid was collected by filtration, washed with MeOH and dried in vacuo. This allowed the isolation of compound F, 1.33 g (32%).

출처