反应详情

温度

120 °C

A mixed solution of 45.0 g of 1-bromopyrene, 21.7 g of 4-methylphenylboronic acid, 34.0 g of tripotassium phosphate, 10.3 g of tetrabutylammonium bromide, 0.71 g of palladium acetate and 1.6 L of dimethylformamide was heated with stirring under a nitrogen gas flow at 120° C. for 5 hours. After cooling to room temperature, 1.6 L of water was injected, followed by stirring at room temperature for 0.5 hours. The precipitated solid was collected by filtration and then washed twice with 200 ml of water. The resultant solid was dissolved in 500 ml of dichloromethane, dried over magnesium sulfate, evaporated and then filtered using Celite. The filtrate was evaporated and the residue was washed twice with 200 ml of methanol. The precipitated solid was collected by filtration and then vacuum-dried to obtain 40.0 g of 1-(4-methylphenyl)pyrene.

1. temperatureAfter cooling to room temperature
2. stirringby stirring at room temperature for 0.5 hours
3. filtrationThe precipitated solid was collected by filtration
4. washwashed twice with 200 ml of water
5. dissolutionThe resultant solid was dissolved in 500 ml of dichloromethane
6. dry with materialdried over magnesium sulfate
7. customevaporated
8. filtrationfiltered
9. customThe filtrate was evaporated
10. washthe residue was washed twice with 200 ml of methanol
11. filtrationThe precipitated solid was collected by filtration
12. customvacuum-dried