反应详情

1.6 g of hexabromospirobifluorene and 3 g of biphenylboronic acid were suspended in a mixture of 50 ml of toluene and 50 ml of 1 M potassium carbonate solution in a 250 ml two-necked flask with a reflux condenser and precision glass stirrer. The mixture was boiled under reflux under nitrogen, and 115 mg of tetrakis(triphenylphosphine)palladium in 5 ml of toluene were added. The mixture was boiled under reflux for 7 hours, while stirring. When the reaction had ended, the cooled solution was filtered off and the filtrate was extracted 2× by shaking with water (chloroform was added for better phase separation). The organic phase was dried over sodium sulfate and filtered over a short column with silica gel and the solvent was then stripped off on a rotary evaporator. For further purification, the product was recrystallized from methylene chloride/pentane. 2 g (80%) of colorless crystals which fluoresce blue under UV illumination were obtained.

1. temperatureunder reflux under nitrogen
2. temperatureunder reflux for 7 hours
3. filtrationthe cooled solution was filtered off
4. extractionthe filtrate was extracted 2×
5. stirringby shaking with water (chloroform
6. additionwas added for better phase separation)
7. dry with materialThe organic phase was dried over sodium sulfate
8. filtrationfiltered over a short column with silica gel
9. customthe solvent was then stripped off on a rotary evaporator
10. customFor further purification
11. customthe product was recrystallized from methylene chloride/pentane
12. customwere obtained