反応 #6884

反応方程式

2-iodotoluene

N-(2-propynyl)piperidine

→

oil

収率 62.3%

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

収率 62.3%

溶媒

diethylamine

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度under reflux for 5 hours
3. 3
   その他The solvent was removed under reduced pressure
4. 4
   洗浄washed with water
5. 5
   乾燥The organic phase was dried over magnesium sulfate
6. 6
   濃縮concentrated completely under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

実験手順

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.

出典