反应详情

A degassed solution of 30 g (86.6 mmol) of 3-bromo-8H-8,12b-diazabenzo-[a]aceanthrylene and 8.8 g (95.9 mmol) of phenylamine in 1 l of dioxane is saturated with N2 for 1 h. Then, firstly 0.9 ml (4.3 mmol) of P(tBu)3, then 0.480 g (2.1 mmol) of palladium acetate are added to the solution. 12.6 g (131 mmol) of NaOtBu in the solid state are subsequently added. The reaction mixture is heated under reflux for 18 h. After cooling to room temperature, 1 l of water is carefully added. The organic phase is washed with 4×50 ml of H2O and dried over MgSO4, and the solvents are removed in vacuo. The pure product is obtained by recrystallisation. The yield is 27 g (64 mmol), corresponding to 76% of theory.

1. temperatureThe reaction mixture is heated
2. temperatureunder reflux for 18 h
3. washThe organic phase is washed with 4×50 ml of H2O
4. dry with materialdried over MgSO4
5. customthe solvents are removed in vacuo
6. customThe pure product is obtained by recrystallisation