Reaktion #308358

Reaktionsgleichung

3-pyridine boronic acid

sodium carbonate

toluene

2,5-dibromopyridine

→

5-bromo-2,3′-bipyridine

Ausbeute 70.6%

Lösungsmittel

water

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux temperature for 3.5 hours
2. 2
   TemperaturAfter heating
3. 3
   Sonstigethe reaction liquid
4. 4
   Extraktionthe organic layer was extracted
5. 5
   EinengenThe organic layer was concentrated in an evaporator
6. 6
   Sonstigethe concentrates were purified by column chromatography
7. 7
   Sonstigerecrystallized in heptane

Vorschrift

Into a 11 flask, 20 g of 3-pyridine boronic acid, 50 g of 2,5-dibromopyridine, 5.5 g of Pd(PPh3)4, 33.9 g of sodium carbonate, 500 ml of toluene, 150 ml of ethanol, and 150 ml of pure water were put, and the solution was stirred at reflux temperature for 3.5 hours. After heating, the reaction liquid was cooled to room temperature and the organic layer was extracted. The organic layer was concentrated in an evaporator, the concentrates were purified by column chromatography, then, recrystallized in heptane, and thus 27 g of 5-bromo-2,3′-bipyridine was obtained.

Quelle