反应详情

913 mg (3 mmol) of tri-o-tolylphosphine and then 112 mg (0.5 mmol) of palladium(II) acetate are added to a vigorously stirred suspension of 14.8 g (50 mmol) of 9-bromobenzimidazo[2,1-a]isoquinoline, 9.9 g (55 mmol) of 1,1′-biphenyl-2-boronic acid and 25.5 g (120 mmol) of tri-potassium phosphate in a mixture of 300 ml of toluene, 100 ml of dioxane and 400 ml of water, and the mixture is subsequently heated under reflux for 16 h. After cooling, the precipitated solid is filtered off with suction, washed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v), three times with 100 ml of ethanol and finally dried. The residue is recrystallised from toluene. The yield is 17 g (45 mmol, 92%).

1. temperaturethe mixture is subsequently heated
2. temperatureunder reflux for 16 h
3. temperatureAfter cooling
4. filtrationthe precipitated solid is filtered off with suction
5. washwashed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v), three times with 100 ml of ethanol
6. customfinally dried
7. customThe residue is recrystallised from toluene