反応 #721740

反応方程式

tri-tert-butylphosphine

9,9″-diphenyl-9H,9′H,9″H-[3,3′;6′,3″]tercarbazole

9,9″-Diphenyl-9H,9′H,9″H-[3,3′;6′,3″]tercarbazole

2-(3-bromophenyl)-4,6-diphenylpyrimidine

NaOtBu

→

9′-[3-(4,6-Diphenylpyrimidin-2-yl)phenyl]-9,9″-diphenyl-9H,9′H,9″H-[3,3′;6′,3″]tercarbazole

溶媒

p-xylene

反応条件

後処理

1. 1
   温度The reaction mixture is heated
2. 2
   温度under reflux for 19 h
3. 3
   温度After cooling
4. 4
   その他the organic phase is separated off
5. 5
   洗浄washed three times with 100 ml of water
6. 6
   その他subsequently evaporated to dryness
7. 7
   抽出The residue is extracted with hot toluene
8. 8
   その他recrystallised from toluene

実験手順

28.8 g (44.32 mmol) of 9,9″-diphenyl-9H,9′H,9″H-[3,3′;6′,3″]tercarbazole 29, 18.88 g (48.76 mmol) of 2-(3-bromophenyl)-4,6-diphenylpyrimidine 14 and 13.01 g (135.35 mmol) of NaOtBu are suspended in 820 ml of p-xylene. 201.21 mg (0.90 mmol) of Pd(OAc)2 and 2.7 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 toluene, recrystallised from toluene and finally sublimed in a high vacuum. The yield is 23.3 g (55%).

出典