反应 #806233

反应方程式

12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole

4-bromobiphenyl

sodium bisulfite

3,5-di(tert-butyl)salicylic acid

potassium carbonate

dodecylbenzene

→

10-(biphenyl-4-yl)-12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole

收率 88.9%

溶剂

toluene

反应条件

后处理

1. 1
   温度heated
2. 2
   温度After cooled to 120° C.
3. 3
   workup.STIRRINGthe mixture was stirred
4. 4
   过滤a crude product was collected by filtration
5. 5
   workup.ADDITIONAfter adding toluene (1.6 L) to the crude product
6. 6
   温度the crude product was heated
7. 7
   萃取extracted at 110° C
8. 8
   温度After cooled to a room temperature
9. 9
   浓缩the crude product was concentrated under reduced pressure
10. 10
    其他The product was crystallized with methanol (120 ml)

实验过程

12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole synthesized in Example 1 (35.5 g), 4-bromobiphenyl (35.0 g), sodium bisulfite (6.0 g), a copper powder (2.4 g), 3,5-di(tert-butyl)salicylic acid (9.4 g), potassium carbonate (31.2 g), and dodecylbenzene (52 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 190° C. for 26 hours. After cooled to 120° C., the mixture was stirred after adding toluene (35 ml), and a crude product was collected by filtration. After adding toluene (1.6 L) to the crude product, the crude product was heated and extracted at 110° C. After cooled to a room temperature, the crude product was concentrated under reduced pressure. The product was crystallized with methanol (120 ml) to obtain a white powder of 10-(biphenyl-4-yl)-12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole (48.5 g; yield 88.1%).

来源