反应详情

19.55 g (53.97 mmol) of 7-bromo-12,12-dimethyl-10,12-dihydro-10-aza-indeno[2,1-b]fluorene 19, 22.99 g (59.37 mmol) of 2-(3-bromophenyl)-4,6-diphenylpyrimidine 14 and 15.84 g (164.81 mmol) of NaOtBu are suspended in 820 ml of p-xylene. 245.0 mg (1.09 mmol) of Pd(OAc)2 and 3.3 ml of a 1M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 19 h. After cooling, the organic phase is separated off, washed three times with 100 ml of water and subsequently evaporated to dryness. The residue is extracted with hot tolu-ene, recrystallised from toluene. The yield is 21.65 g (65%).

1. temperatureThe reaction mixture is heated
2. temperatureunder reflux for 19 h
3. temperatureAfter cooling
4. customthe organic phase is separated off
5. washwashed three times with 100 ml of water
6. customsubsequently evaporated to dryness
7. extractionThe residue is extracted with hot tolu-ene
8. customrecrystallised from toluene