반응 #2364529

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
   workup.ADDITIONare subsequently added
2. 2
   온도The reaction mixture is heated
3. 3
   온도under reflux for 18 h
4. 4
   세척The organic phase is washed with 4×50 ml of water
5. 5
   건조dried over MgSO4
6. 6
   기타the solvent is removed in vacuo
7. 7
   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 1000 ml dioxane is saturated with N2 for 1 h. Then firstly 0.9 ml (4.3 mmol) of P(tBu)3, then 0.48 g (2.1 mmol) of palladium(II) acetate are added to the solution, and 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, 1000 ml of water are carefully added. The organic phase is washed with 4×50 ml of water and dried over MgSO4, and the solvent is removed in vacuo. The pure product is obtained by recrystallisation.

출처