反応 #6886

反応方程式

3-fluoroiodobenzene

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

→

oil

収率 56.2%

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

収率 56.2%

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
   その他the solvent was removed under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

実験手順

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.

出典