反応 #1340562

反応方程式

o-terphenyl

K2CO3

water

→

triphenylene

収率 35.0%

溶媒

DMA

反応条件

後処理

1. 1
   温度The reaction mixture is cooled
2. 2
   抽出extracted with dichloromethane
3. 3
   その他The organic phase is dried
4. 4
   その他the solvent is removed under reduced pressure
5. 5
   その他the residue is purified by means of a short silica gel column (dichloromethane)

実験手順

2.87 mmol of the o-terphenyl derivative, 0.14 mmol of Pd(OAc)2 and 5.7 mmol of K2CO3 are heated in 7 ml of DMA at 135° C. for 24 hours under a nitrogen atmosphere. The reaction mixture is cooled, treated with 5 ml of water and extracted with dichloromethane. The organic phase is dried, the solvent is removed under reduced pressure and the residue is purified by means of a short silica gel column (dichloromethane). After column chromatography (dichloromethane/hexane, 2:1), the desired triphenylene derivative (IIa) is obtained in from 35 to 40% yield.

出典