Reaktion #92813

ord-b1a99e4574d64a38801f876484d345f0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturto reflux for 16 h
  3. 3
    SonstigeAfter the completion of reaction
  4. 4
    Sonstigethe reaction was quenched with water
  5. 5
    ExtraktionThe reaction mixture was then extracted
  6. 6
    Trocknenand the organic layer was dried over anhydrous sodium sulfate
  7. 7
    Sonstigeevaporated to dryness under vacuum

Vorschrift

Indolo[2,3-a]carbazole (9.8 g) was dissolved in 150 ml of dry toluene under nitrogen. 12.9 g of 3-bromo-p-terphenyl, 0.65 g of tris(dibenzylideneacetone) dipalladium, 0.46 g of tri-t-butylphosphine and 40.3 g of potassium orthophosphate were added and heated to reflux for 16 h. After the completion of reaction, the reaction was quenched with water. The reaction mixture was then extracted using ethyl acetate; and the organic layer was dried over anhydrous sodium sulfate and evaporated to dryness under vacuum. Subsequent silica gel column chromatography using ethyl acetate/hexane (1:9) as eluent, yielded 12.6 g of N-(1,1′:4′,1″-terphenyl-3-yl)indolo[2,3-a]carbazole.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09450192B2uspto-grants-2016_09