反应详情

In a 200 mL three-neck flask, 5.2 g (23 mmol) of 9-anthrylboronic acid, 4.0 g (25 mmol) of 3-bromopyridine, 5.2 g (50 mmol) of sodium carbonate, 50 mL of toluene, 25 μL of ethanol, and 25 mL of water were placed. The mixture was degassed by being stirred under reduced pressure, and the air in the flask was replaced with nitrogen. To the mixture, 0.28 g (0.25 mmol) of tetrakis(triphenylphosphine)palladium(0) was added, and the mixture was stirred under nitrogen stream at 80° C. for 7 hours. After a certain period, water was added to the mixture, and an aqueous layer was extracted with toluene. The obtained extracted solution and the organic layer were combined, washed with saturated saline, and dried with magnesium sulfate. The obtained mixture was gravity filtered, and the filtrate was condensed to give an oily substance. The oily substance was recrystallized with toluene/hexane, so that 2.8 g of target yellow powder was obtained in a yield of 46%.

1. customThe mixture was degassed
2. stirringthe mixture was stirred under nitrogen stream at 80° C. for 7 hours
3. waitAfter a certain period
4. extractionan aqueous layer was extracted with toluene
5. extractionThe obtained extracted solution
6. washwashed with saturated saline
7. dry with materialdried with magnesium sulfate
8. filtrationfiltered
9. customcondensed
10. customto give an oily substance
11. customThe oily substance was recrystallized with toluene/hexane, so that 2.8 g of target yellow powder
12. customwas obtained in a yield of 46%