تفاعل #308361

معادلة التفاعل

THF

2,6-dibromopyridine

normal-butyllithium

3-bromopyridine

→

6-bromo-2,3′-bipyridine

المردود 44.7%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was heated to room temperature
2. 2
   أخرىThe reaction liquid
3. 3
   غسيلwas washed by an ammonium chloride aqueous solution
4. 4
   تركيزthe organic layer was concentrated in an evaporator
5. 5
   أخرىThe concentrates were purified by column chromatography

الإجراء التجريبي

Under nitrogen atmosphere, 6.32 g of 3-bromopyridine was dissolved in 400 ml of dehydrated toluene. The solution was cooled at −78° C. and 17 ml of 2.6M normal-butyllithium was dropped. After 0.5 hours, 12.6 g of zinc chloride tetramethylethylenediamine, and 200 ml of dehydrated THF were added. The solution was heated to room temperature, 10.63 g of 2,6-dibromopyridine and 0.6 g of Pd(PPh3)4 were added, and the solution was stirred for 24 hours. The reaction liquid was washed by an ammonium chloride aqueous solution, and the organic layer was concentrated in an evaporator. The concentrates were purified by column chromatography, and thus 4.2 g of 6-bromo-2,3′-bipyridine was obtained.

المصدر