反应详情

温度

60 °C

190 μl (1 mmol) of chloro-di-tert-butylphosphine and then 112 mg (0.5 mmol) of palladium(II) acetate are added to a suspension of 15.4 g (50 mmol) of 4-bromobenz[a]anthracene, 11.8 g (60 mmol) of bis(3-methylphenyl)amine and 7.7 g (80 mmol) of sodium tert-butoxide in 500 ml of toluene, and the mixture is subsequently heated under reflux for 5 h. After the mixture has been cooled to 60° C., 500 ml of water are added, the organic phase is separated off, filtered through silica gel, evaporated virtually to dryness at 80° C. in vacuo, and 300 ml of ethanol are then added. After cooling, the solid is filtered off with suction. Recrystallisation five times from dioxane (about 8 ml/g); sublimation (p=5×10−5 mbar, T=280° C.). Yield: 11.9 g (28 mmol), 56.1%, purity 99.9% (HPLC).

1. temperaturethe mixture is subsequently heated
2. temperatureunder reflux for 5 h
3. customthe organic phase is separated off
4. filtrationfiltered through silica gel
5. customevaporated virtually to dryness at 80° C. in vacuo, and 300 ml of ethanol
6. additionare then added
7. temperatureAfter cooling
8. filtrationthe solid is filtered off with suction
9. customRecrystallisation five times from dioxane (about 8 ml/g)
10. customsublimation (p=5×10−5 mbar, T=280° C.)