反应详情

2.25 g (6.3 mmol) of 4,4,5,5-tetramethyl-2-(triphenylen-2-yl)-1,3,2-dioxaborolane, 0.92 g (2.7 mmol) of 2,8-dibromodibenzothiophene, 0.12 g (0.14 mmol) of Pd2(dba)3, 0.22 g (0.53 mmol) of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl, 3.4 g (16.0 mmol) of K3PO4, 100 mL of toluene and 10 mL of water were charged in a 250 mL round bottom flask. The reaction mixture was purged with nitrogen for 20 min and then heated up to reflux for overnight with stirring. The reaction mixture was cooled and filtered. The white solid was washed with methanol 3 times (3×100 mL) and methylene chloride (2×100 mL). 1.6 g of (94% yield) solid was obtained as the product which was further purified by recrystallization with toluene and sublimation. The product was confirmed by solid probe MS.

1. customThe reaction mixture was purged with nitrogen for 20 min
2. temperatureheated up
3. temperatureto reflux for overnight
4. temperatureThe reaction mixture was cooled
5. filtrationfiltered
6. washThe white solid was washed with methanol 3 times (3×100 mL) and methylene chloride (2×100 mL)