Реакция #6884

Уравнение реакции

2-iodotoluene

N-(2-propynyl)piperidine

→

oil

Выход 62.3%

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

Выход 62.3%

Растворители

diethylamine

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураunder reflux for 5 hours
3. 3
   ДругоеThe solvent was removed under reduced pressure
4. 4
   Промывкаwashed with water
5. 5
   СушкаThe organic phase was dried over magnesium sulfate
6. 6
   Концентрированиеconcentrated completely under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

Методика

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.

Источник