Reaktion #6884

Reaktionsgleichung

2-iodotoluene

N-(2-propynyl)piperidine

→

oil

Ausbeute 62.3%

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

Ausbeute 62.3%

Lösungsmittel

diethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 5 hours
3. 3
   SonstigeThe solvent was removed under reduced pressure
4. 4
   Waschenwashed with water
5. 5
   TrocknenThe organic phase was dried over magnesium sulfate
6. 6
   Einengenconcentrated completely under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

Vorschrift

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.

Quelle