反应详情

10 g (19.4 mmol) of 10-(4′-bromobiphenyl-4-yl)-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene are dissolved in 300 ml of toluene with 9.6 g (30 mmol) of bis(4-biphenylyl)amine and degassed. 1.94 ml (1.94 mmol/1 M in toluene) of tri-tert-butylphosphine, 252 mg of Pd(OAc)2 and 4.1 g (41.7 mmol) of NaOt-Bu are added, and the mixture is stirred under reflux for 10 h. The mixture is filtered through Alox B (activity grade 1), washed with water, dried and evaporated. The crude product is extracted with toluene in a Soxhlet extractor, recrystallised from toluene/heptane, giving 6.7 g (8.9 mmol, 46%) of the product as a yellow solid. Finally, the product is sublimed in a high vacuum, the purity is 99.9%.

1. customdegassed
2. temperatureunder reflux for 10 h
3. filtrationThe mixture is filtered through Alox B (activity grade 1)
4. washwashed with water
5. customdried
6. customevaporated
7. extractionThe crude product is extracted with toluene in a Soxhlet extractor
8. customrecrystallised from toluene/heptane