Reaktion #610222

ord-7e2f9e5bdb804252aafb4477ccce91da

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is subsequently heated
  2. 2
    Temperaturunder reflux for 16 h
  3. 3
    TemperaturAfter cooling
  4. 4
    Filtrationthe precipitated solid is filtered off with suction
  5. 5
    Waschenwashed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v) and three times with 100 ml of ethanol
  6. 6
    Sonstigerecrystallised three times from DMF (about 15 ml/g)

Vorschrift

2.47 g (8.1 mmol) of tetrakistriphenylphosphinopalladium(0) are added to a vigorously stirred suspension of 6.8 g (20 mmol) of 3,6-dibromodibenzothiophene, 15 g (40 mmol) of 9-phenyl-9H-carbazole-3-boronic acid and 63.9 g (127 mmol) of Na2CO3 in 500 ml of DMF, and the mixture is subsequently heated under reflux for 16 h. After cooling, the precipitated solid is filtered off with suction, washed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v) and three times with 100 ml of ethanol and recrystallised three times from DMF (about 15 ml/g). Yield 17.4 g (33 mmol), 86.0%, purity 99.9% (HPLC).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09334260B2uspto-grants-2016_05