Reaktion #308364

Reaktionsgleichung

9,9-dihexyl-fluorene-2,7-diboronic acid

5-bromo-2,3′-bipyridine

tripotassium phosphate

→

2,7-bis(2,3′-bipyridine-5-yl)-9,9-dihexylfluorene

Ausbeute 32.8%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux temperature for 6.5 hours under argon atmosphere
2. 2
   TemperaturAfter heating
3. 3
   Sonstigethe reaction liquid
4. 4
   Waschenwashed by a saturated sodium chloride aqueous solution
5. 5
   EinengenThe organic layer was concentrated in an evaporator
6. 6
   Sonstigethe concentrates were purified by activated alumina column chromatography
7. 7
   SonstigeThe concentrates were recrystallized in a heptane/ethyl acetate mixed solvent

Vorschrift

Into a flask, 0.6 g of 9,9-dihexyl-fluorene-2,7-diboronic acid, 0.5 g of 5-bromo-2,3′-bipyridine, 115 mg of Pd(PPh3)4, 1.27 g of tripotassium phosphate, and 20 ml of toluene were put, and the solution was stirred at reflux temperature for 6.5 hours under argon atmosphere. After heating, the reaction liquid was cooled to room temperature, and washed by a saturated sodium chloride aqueous solution. The organic layer was concentrated in an evaporator, and the concentrates were purified by activated alumina column chromatography. The concentrates were recrystallized in a heptane/ethyl acetate mixed solvent, and thus 150 mg of 2,7-bis(2,3′-bipyridine-5-yl)-9,9-dihexylfluorene was obtained.

Quelle