تفاعل #6884

ord-0f8d0671097c4c1fb7b5e5e1778ceb8b

معادلة التفاعل

Cc1ccccc1I
2-iodotoluene
C#CCN1CCCCC1
N-(2-propynyl)piperidine
Cc1ccccc1C#CCN1CCCCC1
oil
المردود 62.3%
Cc1ccccc1C#CCN1CCCCC1
1-(3-o-Tolyl-2-propynyl)piperidine
المردود 62.3%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux for 5 hours
  3. 3
    أخرىThe solvent was removed under reduced pressure
  4. 4
    غسيلwashed with water
  5. 5
    تجفيفThe organic phase was dried over magnesium sulfate
  6. 6
    تركيزconcentrated completely under reduced pressure
  7. 7
    workup.DISTILLATIONDistillation of the residue under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07084158B2uspto-grants-2006_08