반응 #1340561

반응 방정식

Na2CO3

toluene

→

o-terphenyl

수율 40.0%

반응 조건

후처리

1. 1
   온도the mixture is heated up
2. 2
   온도to reflux under nitrogen
3. 3
   온도The reaction mixture is heated
4. 4
   온도under reflux for 6 hours
5. 5
   온도cooled
6. 6
   기타the phases formed
7. 7
   기타are separated
8. 8
   추출the water phase is extracted with dichloromethane
9. 9
   기타dried
10. 10
    기타The solvent is removed under reduced pressure
11. 11
    기타the crude product is purified by means of a short silica gel column
12. 12
    기타After purification by column chromatography (dichloromethane/hexane, 2:1)

실험 절차

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.

출처