반응 #6884

반응 방정식

2-iodotoluene

N-(2-propynyl)piperidine

→

oil

수율 62.3%

1-(3-o-Tolyl-2-propynyl)piperidine

수율 62.3%

용매

diethylamine

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 5 hours
3. 3
   기타The solvent was removed under reduced pressure
4. 4
   세척washed with water
5. 5
   건조The organic phase was dried over magnesium sulfate
6. 6
   농축concentrated completely under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

실험 절차

A mixture of 2-iodotoluene (6.54 g), N-(2-propynyl)piperidine (3.69 g), dichlorobis(triphenylphosphino)palladium(II) (0.05 g) and copper(I) iodide (0.1 g) in dry diethylamine (50 ml) was heated under reflux for 5 hours. The solvent was removed under reduced pressure and the residue was taken up in diethyl ether and washed with water. The organic phase was dried over magnesium sulfate and concentrated completely under reduced pressure. Distillation of the residue under reduced pressure gave 3.98 g of an oil of boiling point 96–98° C./0.08 mm Hg.

출처