反应详情

温度

68 °C

2-Bromo-9,9-dimethyl-7,10-diphenylacridan (2.54 g), 4-(diphenylamino)phenylboronic acid (1.75 g), toluene (25 ml), ethanol (2 ml), and a 2M potassium carbonate aqueous solution (9 ml) were added to a reaction vessel in a nitrogen atmosphere and aerated with nitrogen gas for 30 min under ultrasonic irradiation. The mixture was heated after adding tetrakis(triphenylphosphine)palladium (0.20 g) and stirred at 68° C. for 8 hours. The mixture was allowed to cool to a room temperature, and an organic layer was collected by a liquid separating operation. The organic layer was dried with magnesium sulfate and concentrated under reduced pressure to obtain a yellow amorphous crude product. The crude product was recrystallized with n-hexane, dissolved by adding toluene (30 ml), and purified by adsorption using silica gel (1.17 g Methanol (20 ml) was added to this solution to precipitate crystals, and the crystals were further purified by recrystallization using toluene/methanol to obtain a white powder of [4-(9,9-dimethyl-7,10-diphenylacridan-2-yl)phenyl]-diphenylamine (1.9 g; yield 54%).

1. temperatureThe mixture was heated
2. temperatureto cool to a room temperature
3. customan organic layer was collected by a liquid
4. customseparating operation
5. dry with materialThe organic layer was dried with magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customto obtain a yellow amorphous crude product
8. customThe crude product was recrystallized with n-hexane
9. dissolutiondissolved
10. additionby adding toluene (30 ml)
11. custompurified by adsorption
12. additionwas added to this solution
13. customto precipitate crystals
14. customthe crystals were further purified by recrystallization