반응 #75609

반응 방정식

1-benzyl-4-piperidinecarbonitrile

1-chloroethyl chloroformate

→

4-piperidinecarbonitrile hydrochloride

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   온도under ice-cooling
2. 2
   온도heated
3. 3
   온도under reflux for 1 hr and 20 min
4. 4
   기타After evaporating
5. 5
   workup.ADDITION50 ml methanol was added
6. 6
   온도it was heated
7. 7
   온도under reflux for 1 hr
8. 8
   기타The reaction solution was evaporated
9. 9
   세척the crystalline residue was washed with ethyl acetate
10. 10
    여과collected by filtration

실험 절차

11.0 g of 1-benzyl-4-piperidinecarbonitrile was dissolved in 100 ml 1,2-dichloroethane, 7.1 ml 1-chloroethyl chloroformate was added thereto under ice-cooling. The mixture was stirred at room temperature for 15 min, and then heated under reflux for 1 hr and 20 min. After evaporating, 50 ml methanol was added thereto and it was heated under reflux for 1 hr. The reaction solution was evaporated, and the crystalline residue was washed with ethyl acetate and collected by filtration to give 8.0 g of 4-piperidinecarbonitrile hydrochloride as white crystals.

출처