反应 #806237

反应方程式

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

2-bromo-9,9-dimethyl-9H-fluorene

sodium bisulfite

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

potassium carbonate

dodecylbenzene

→

12,12-dimethyl-10-(9,9-dimethyl-9H-fluorene-2-yl)-10,12-dihydroindeno[2,1-b]carbazole

收率 80.2%

反应条件

后处理

1. 1
   温度heated
2. 2
   温度The mixture was cooled to 100° C.
3. 3
   其他insoluble matter was removed by filtration
4. 4
   workup.ADDITIONafter adding toluene (80 ml)
5. 5
   浓缩a filtrate was concentrated
6. 6
   其他Crystallization

实验过程

12,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole synthesized in Example 1 (5.5 g), 2-bromo-9,9-dimethyl-9H-fluorene (6.4 g), sodium bisulfite (0.3 g), a copper powder (0.1 g), 3,5-di(tert-butyl)salicylic acid (0.5 g), potassium carbonate (4.0 g), and dodecylbenzene (5 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 180° C. for 29 hours. The mixture was cooled to 100° C., and insoluble matter was removed by filtration after adding toluene (80 ml), and a filtrate was concentrated. Crystallization using n-hexane (20 ml) was performed to obtain an ocher powder of 12,12-dimethyl-10-(9,9-dimethyl-9H-fluorene-2-yl)-10,12-dihydroindeno[2,1-b]carbazole (7.4 g; yield 80.0%)

来源