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
- 205 °C
PROCEDURE
实验过程
Indane-5-yl-p-tolylamine (18.1 g (0.081 mol)), 18.9 g (0.039 mol) of 4,4″-diiodo-p-terphenyl, 7.2 g (0.052 mol) of anhydrous potassium carbonate, 0.76 g (0.012 mol) of copper powder and 30 ml of n-dodecane were mixed, and heated up to 200 to 210° C. while introducing nitrogen gas, followed by stirring for 30 hours. After the termination of the reaction, the reaction product was extracted with 400 ml of toluene, and insoluble matter was removed by filtration. Then, the filtrate was concentrated to dryness. The resulting solid matter was purified by column chromatography (carrier: silica gel, eluent: toluene:hexane=1:4) to obtain 19.9 g of N,N′-bisindane-5-yl-N,N′-di-p-tolyl-4,4″-diamino-p-terphenyl (compound No. 1) (yield: 75.7%, melting point: 207.4 to 208.1° C.).
WORKUP
后处理
- additionwhile introducing nitrogen gas
- customAfter the termination of the reaction
- extractionthe reaction product was extracted with 400 ml of toluene, and insoluble matter
- customwas removed by filtration
- concentrationThen, the filtrate was concentrated to dryness
- customThe resulting solid matter was purified by column chromatography (carrier: silica gel, eluent: toluene:hexane=1:4)