反应详情

4,4′-Iminobis(biphenyl) (2.0 g, 6.23 mmol), and 4,4′-dibromobiphenyl (3.9 g, 12.6 mmol) were mixed in 150 mL of anhydrous toluene. To the solution was bubbled nitrogen while stirring for 15 min. Pd(OAc)2 (0.02 g, 0.089 mmol), triphenylphosphine (0.09 g, 0.34 mmol) and tBuONa (1.15 g, 11.9 mmol) were added in sequence. The mixture was heated to reflux overnight under nitrogen. After cooling, the reaction mixture was filtered through Celite pad and the solvent was then evaporated. The residue (3.1 g, 90%) was recrystallized by toluene and the crystal was further purified by boiling with 15 ml degassed toluene, 2.7 g (78%) of the desired compound was collected.

1. customTo the solution was bubbled nitrogen
2. temperatureThe mixture was heated
3. temperatureto reflux overnight under nitrogen
4. temperatureAfter cooling
5. filtrationthe reaction mixture was filtered through Celite pad
6. customthe solvent was then evaporated
7. customThe residue (3.1 g, 90%) was recrystallized by toluene
8. customthe crystal was further purified
9. customdegassed toluene, 2.7 g (78%) of the desired compound
10. customwas collected