Reaktion #805176

ord-373797317bbe4301a53ec9f78b8163fc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was degassed
  2. 2
    Sonstigeby bubbling N2 for 30 minutes
  3. 3
    Temperaturheated
  4. 4
    Temperaturto reflux under N2 overnight
  5. 5
    Sonstigethe crude product was purified by silica gel column
  6. 6
    Sonstigeto yield 3.3 g (99%), which

Vorschrift

4-iododibenzo[b,d]furan (4 g, 13.60 mmol), phenylboronic acid (1.99 g, 16.32 mmol), dicyclohexyl(2′,6′-dimethoxy-[1,1′-biphenyl]-2-yl)phosphine (0.447 g, 1.08 mmol), Pd2(dba)2 (0.250 g, 0.272 mmol), K3PO4 (10.1 g, 47.6 mmol), 150 mL toluene and 15 mL water were charged in a 250 mL flask. The reaction mixture was degassed by bubbling N2 for 30 minutes and then heated to reflux under N2 overnight. The reaction was cooled to room temperature and the crude product was purified by silica gel column to yield 3.3 g (99%), which was confirmed by GC-MS.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09193745B2uspto-grants-2015_11