反应详情

Xylene (250 mL) was bubbled with nitrogen for 15 min, followed by addition of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (1.8 g, 4.4 mmol) and Pd2(dba)3 (1.0 g, 1.1 mmol). The mixture was bubbled with nitrogen for 15 min, then [1,1′:3′,1″-terphenyl]-4′-amine (9.8 g, 40.0 mmol), 4-iodobiphenyl (10.3 g, 36.7 mmol), sodium tert-butoxide (7.0 g, 73.4 mmol) were added. The mixture was bubbled with nitrogen for 15 min and refluxed for 13 h. After cooling, the reaction mixture was filtered through a silica pad and washed with toluene. The solvent was removed in vacuo and the residue was purified by flash chromatography using 40-60% toluene/hexane to afford N-([1,1′-biphenyl]-4-yl)-[1,1′:3′,1″-terphenyl]-4′-amine (14.7 g, 92% yield) as a white solid.

1. customXylene (250 mL) was bubbled with nitrogen for 15 min
2. customThe mixture was bubbled with nitrogen for 15 min
3. customThe mixture was bubbled with nitrogen for 15 min
4. temperaturerefluxed for 13 h
5. temperatureAfter cooling
6. filtrationthe reaction mixture was filtered through a silica pad
7. washwashed with toluene
8. customThe solvent was removed in vacuo
9. customthe residue was purified by flash chromatography