تفاعل #748994

ord-fcbc2aaf753643d6aa7d9fc0c3acceb3

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةunder reflux for 30 hr
  3. 3
    درجة الحرارةto cool
  4. 4
    ترشيحthe mixture was filtered
  5. 5
    workup.DISTILLATIONThe solvent in the filtrate was distilled off under reduced pressure
  6. 6
    workup.ADDITIONMethanol (500 ml) was added to the residue
  7. 7
    أخرىto precipitate crystals
  8. 8
    ترشيحThe crystals were collected by filtration

الإجراء التجريبي

A 2-L Kolben equipped with a stirrer and a drain device was charged under a nitrogen stream with 150 g (369.5 mmol) of 4,4′-diiodobiphenyl, 123.5 g (738.6 mmol) of carbazole, 23 g of copper powder, 100 g of potassium carbonate, and 500 ml of 1,3-diisopropylbenzene. The mixture was heated under reflux for 30 hr and was allowed to cool. Toluene was then added, and the mixture was filtered. The solvent in the filtrate was distilled off under reduced pressure. Methanol (500 ml) was added to the residue to precipitate crystals. The crystals were collected by filtration to give CBP (4,4′-bis(carbazol-9-yl)-biphenyl) (122.8 g, yield 68.6%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08084935B2uspto-grants-2011_12