反应 #6886

反应方程式

3-fluoroiodobenzene

4-methyl-1-(2-propynyl)piperidine

→

oil

收率 56.2%

1-[3-(3-Fluorophenyl)-2-propynyl]-4-methylpiperidine

收率 56.2%

溶剂

diethylamine

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度under reflux for 5 hours
3. 3
   其他The solvent was removed under reduced pressure
4. 4
   洗涤washed with water
5. 5
   干燥The organic phase was dried over magnesium sulfate
6. 6
   其他the solvent was removed under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

实验过程

A mixture of 3-fluoroiodobenzene (8.88 g), 4-methyl-1-(2-propynyl)piperidine (6.80 g), palladium acetate (0.045 g), tri-o-toloylphosphine (0.24 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 the solvent was removed under reduced pressure. Distillation of the residue under reduced pressure gave an oil (5.20 g) of boiling point 105° C./0.07 mm Hg.

来源