反応 #610219

反応方程式

2-phenylcarbazole

3,6-dibromo-9-(phenylsulfonyl)-9H-carbazole

potassium phosphate

→

3,3″-Bis(phenyl)-9′-[(phenyl)sulfonyl]-9,3′:6′,9″-ter-9H-carbazole

溶媒

dioxane

反応条件

後処理

1. 1
   温度the mixture is subsequently heated
2. 2
   温度under reflux for 16 h
3. 3
   温度After cooling
4. 4
   ろ過the precipitated solid is filtered off with suction
5. 5
   洗浄washed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v) and three times with 100 ml of ethanol

実験手順

8.0 g (42.2 mmol) of copper(I) iodide and 11.7 ml (97.5 mmol) of trans-cyclohexanediamine are added to a vigorously stirred suspension of 56.9 g (234 mmol) of 2-phenylcarbazole, 54.4 g (117 mmol) of 3,6-dibromo-9-(phenylsulfonyl)-9H-carbazole and 416.4 g (1961 mmol) of potassium phosphate in 1170 ml of dioxane, and the mixture is subsequently heated under reflux for 16 h. After cooling, the precipitated solid is filtered off with suction, washed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v) and three times with 100 ml of ethanol. Yield: 80 g (101 mmol), 86%.

出典