Реакция #6886

ord-407eb598551c4c3b88f8f45387ed5837

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07084158B2uspto-grants-2006_08