반응 #6886

반응 방정식

3-fluoroiodobenzene

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

→

oil

수율 56.2%

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

수율 56.2%

용매

diethylamine

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 5 hours
3. 3
   기타The solvent was removed under reduced pressure
4. 4
   세척washed with water
5. 5
   건조The organic phase was dried over magnesium sulfate
6. 6
   기타the solvent was removed under reduced pressure
7. 7
   workup.DISTILLATIONDistillation of the residue under reduced pressure

실험 절차

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.

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