반응 #70300

반응 방정식

2,5-dibromopyridine

3-fluoro-4-(tributylstannyl)pyridine

→

expected product

수율 62.0%

5-Bromo-3′-fluoro-2,4′-bipyridine

수율 62.0%

용매

DMF

반응 조건

후처리

1. 1
   기타The solvent was evaporated
2. 2
   추출the crude mixture was extracted between water and ethyl acetate
3. 3
   기타The solid residue was purified by chromatography over SiO2 eluting with DCM/methanol

실험 절차

In a schlenck tube, a mixture of 2,5-dibromopyridine (2.11 mmol, 0.500 g), 3-fluoro-4-(tributylstannyl)pyridine (2.32 mmol, 0.896 g), PdCl2(PPh3)2 (0.21 mmol, 0.148 g), CuI (0.43 mmol, 0.080 g) in DMF (5 ml) was heated at 130° C. for 12 hours, under argon atmosphere. The solvent was evaporated and the crude mixture was extracted between water and ethyl acetate. The solid residue was purified by chromatography over SiO2 eluting with DCM/methanol mixtures affording 0.330 g (yield 62%) of the expected product.

출처