Reaktion #2363130

ord-c2734812dcc3445382cb5863ce3e857c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is heated
  2. 2
    Temperaturunder reflux for 16 h
  3. 3
    TemperaturAfter cooling
  4. 4
    Sonstigethe organic phase is separated off
  5. 5
    Waschenwashed three times with 150 ml of water
  6. 6
    Sonstigesubsequently evaporated to dryness
  7. 7
    SonstigeThe residue is recrystallised from toluene

Vorschrift

7.1 g (9.0 mmol) of 4-(7-bromo-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluoren-10-yl)-4′-(12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluoren-10-yl)biphenyl, 2.5 g (9.85 mmol) of bis(pinacolato)diborane and 2.6 g (26 mmol) of potassium acetate are suspended in 500 ml of dioxane. 0.22 g (0.27 mmol) of 1,1-bis(diphenylphosphino)ferrocenepalladium(II) dichloride complex with dichloromethane is added to this suspension. The reaction mixture is heated under reflux for 16 h. After cooling, the organic phase is separated off, washed three times with 150 ml of water and subsequently evaporated to dryness. The residue is recrystallised from toluene. The yield is 6.8 g (8 mmol, 90%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09126970B2uspto-grants-2015_09