反应详情

A degassed solution of 175 g (400 mmol) of 7-bromo-12,12-dimethyl-10-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene and 67.7 g (401.8 mmol) of p-aminobiphenyl in 1000 ml of toluene is saturated with N2 for 1 h. 2.47 g (4.45 mmol) of 1,1-bis(diphenylphosphino)ferrocene and 1 g (4.45 mmol) of Pd(OAc)2 are then added to the solution, and 50.01 g (521.25 mmol) of NaOtBu in the solid state are subsequently added. The reaction mixture is heated under reflux for 5 h. After cooling to room temperature, 1000 ml of water are added. The organic phase is washed with 4×250 ml of H2O, then dried using MgSO4, and the solvent is removed under reduced pressure. The pure product is obtained by recrystallisation from dioxane as a colourless solid in a yield of 182 g (347 mmol), 87%.

1. additionare subsequently added
2. temperatureThe reaction mixture is heated
3. temperatureunder reflux for 5 h
4. washThe organic phase is washed with 4×250 ml of H2O
5. customdried
6. customthe solvent is removed under reduced pressure
7. customThe pure product is obtained by recrystallisation from dioxane as a colourless solid in a yield of 182 g (347 mmol), 87%