反应 #1340561

反应方程式

Na2CO3

toluene

→

o-terphenyl

收率 40.0%

反应条件

后处理

1. 1
   温度the mixture is heated up
2. 2
   温度to reflux under nitrogen
3. 3
   温度The reaction mixture is heated
4. 4
   温度under reflux for 6 hours
5. 5
   温度cooled
6. 6
   其他the phases formed
7. 7
   其他are separated
8. 8
   萃取the water phase is extracted with dichloromethane
9. 9
   其他dried
10. 10
    其他The solvent is removed under reduced pressure
11. 11
    其他the crude product is purified by means of a short silica gel column
12. 12
    其他After purification by column chromatography (dichloromethane/hexane, 2:1)

实验过程

6.4 mmol of the dibromide (VI) and 6.4 mmol of the arylboronic acid derivative (V) (2-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)pyridine) are dissolved in 25 ml of toluene. 0.4 mmol of Pd(PPh3)4 and 10 ml of a 4N solution of Na2CO3 are added, and the mixture is heated up to reflux under nitrogen. The reaction mixture is heated under reflux for 6 hours and cooled, the phases formed are separated, and the water phase is extracted with dichloromethane and dried. The solvent is removed under reduced pressure and the crude product is purified by means of a short silica gel column. After purification by column chromatography (dichloromethane/hexane, 2:1), the desired o-terphenyl derivative is obtained in from 40 to 50% yield.

来源