반응 #1572771

반응 방정식

P(tBu)3

NaOtBu

3-bromo-8H-8,12b-diazabenzo-[a]aceanthrylene

phenylamine

N2

dioxane

→

Bromo-8-phenyl-8H-8,12b-diazabenzo[a]aceanthrylene

용매

water

반응 조건

후처리

1. 1
   온도The reaction mixture is heated
2. 2
   온도under reflux for 18 h
3. 3
   세척The organic phase is washed with 4×50 ml of H2O
4. 4
   건조dried over MgSO4
5. 5
   기타the solvents are removed in vacuo
6. 6
   기타The pure product is obtained by recrystallisation

실험 절차

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.

출처