反应详情

30 g (106 mmol) of 12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene, 13.3 g (114 mmol) of 5′-bromo-[1,1′;3′,1″]terphenyl and 30.5 g of NaOtBu are suspended in 1.5 l of p-xylene. 0.5 g (2.11 mmol) of Pd(OAc)2 and 1.6 ml of a 1 M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 16 h. After cooling, the organic phase is separated off, washed three times with 200 ml of water and subsequently evaporated to dryness. The residue is extracted with hot toluene, recrystallised from toluene and finally sublimed in a high vacuum, the purity is 99.9%. The yield is 15.8 g (31 mmol, 72%).

1. temperatureThe reaction mixture is heated
2. temperatureunder reflux for 16 h
3. temperatureAfter cooling
4. customthe organic phase is separated off
5. washwashed three times with 200 ml of water
6. customsubsequently evaporated to dryness
7. extractionThe residue is extracted with hot toluene
8. customrecrystallised from toluene