反应 #6884

ord-0f8d0671097c4c1fb7b5e5e1778ceb8b

反应条件

详细条件
See reaction.notes.procedure_details.

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
    浓缩concentrated completely under reduced pressure
  7. 7
    workup.DISTILLATIONDistillation of the residue under reduced pressure

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07084158B2uspto-grants-2006_08