反应详情

N,N-diphenyl-7-bromo-9,9-di-n-decyl-9H-fluorene-2-amine (8.08 9,11.66 mmol), tri-o-tolylphosphine (1.42 g, 4.67 mmol), triethylamine (30 ml, degassed with nitrogen for 15 minutes), 4-vinylpyridine (2.52 ml, 23.32 mmol) and palladium(Il) acetate (0.13 g, 0.58 mmol) were added to a single-necked round bottom flask equipped with a magnetic stirrer and reflux condenser. The solution was heated at reflux by means of an oil bath under nitrogen for 16 hours. The solvent was removed under reduced pressure and the residue dissolved in methylene chloride. The organic layer was washed 3 times with water, dried over anhydrous MgSO4, filtered and concentrated. The product was purified by column chromatography using silica gel and 85:15 hexane:ethyl acetate to afford a yellow oil in 59.45% yield. The oil, upon standing for several days, gradually solidified to give a waxy solid (mp 88.4° C.-89.3° C.). Mass Spec. m/z 716 (M+), 576, (M-C10H20), 358 (M++). Elemental Analysis: Calculated for C52H64N2 : C, 87.10; H, 9.00; N, 3.90. Found: C, 87.17; H, 9.45; N, 3.35.

1. customequipped with a magnetic stirrer
2. temperaturereflux condenser
3. temperatureThe solution was heated
4. temperatureat reflux by means of an oil bath under nitrogen for 16 hours
5. customThe solvent was removed under reduced pressure
6. dissolutionthe residue dissolved in methylene chloride
7. washThe organic layer was washed 3 times with water
8. dry with materialdried over anhydrous MgSO4
9. filtrationfiltered
10. concentrationconcentrated
11. customThe product was purified by column chromatography
12. customethyl acetate to afford a yellow oil in 59.45% yield
13. waitThe oil, upon standing for several days