反応 #617365

反応方程式

1,6-dibromopyrene

phenylboronic acid

sodium carbonate

toluene

→

crude product

1,6-diphenylpyrene

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他to react at 90° C. for 7 hours
2. 2
   温度After cooling
3. 3
   ろ過the reaction solution was filtered
4. 4
   その他solids obtained
5. 5
   洗浄were washed with methanol and clean water
6. 6
   その他Further, the solids were purified by silica gel chromatography (heated toluene)

実験手順

Under an argon atmosphere, 15.0 g of 1,6-dibromopyrene, 13.2 g of phenylboronic acid, 1.9 g of tetrakis(triphenylphosphine)palladium (0) [Pd(PPh3)4], 27.8 g of sodium carbonate (130 mL of clean water), toluene and tetrahydrofuran were placed into a flask, and the resulting mixture was allowed to react at 90° C. for 7 hours. After cooling, the reaction solution was filtered, and solids obtained were washed with methanol and clean water. Further, the solids were purified by silica gel chromatography (heated toluene). The resulting crude product which was obtained by a concentration was re-crystallized from toluene, followed by drying under a reduced pressure, whereby white solids of 1,6-diphenylpyrene (11.8 g) were obtained.

出典