反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 190 °C
PROCEDURE
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%).
WORKUP
后处理
- temperatureheated
- temperatureAfter cooled to 120° C.
- stirringthe mixture was stirred
- filtrationa crude product was collected by filtration
- additionAfter adding toluene (1.6 L) to the crude product
- temperaturethe crude product was heated
- extractionextracted at 110° C
- temperatureAfter cooled to a room temperature
- concentrationthe crude product was concentrated under reduced pressure
- customThe product was crystallized with methanol (120 ml)