反应详情

To a solution of 20.7 g of 2-bromo-6-chloro-4-methylpyridine in 100 ml anhydrous N,N-dimethylformamide 9.9 g of copper cyanide was added. The reaction mixture was heated to reflux for 7 hours. After cooling, the mixture was filtered through a silica gel column with 500 ml ethyl acetate. The obtained solution was washed with a saturated aqueous solution of sodium chloride. The solvent was removed in vacuo and the residue purified by silica gel column chromatography using hexane/ethyl acetate. 1:1. 7.6 g (54%) of the title compound was obtained as a white solid of melting point 133° C.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 7 hours
3. temperatureAfter cooling
4. filtrationthe mixture was filtered through a silica gel column with 500 ml ethyl acetate
5. washThe obtained solution was washed with a saturated aqueous solution of sodium chloride
6. customThe solvent was removed in vacuo
7. customthe residue purified by silica gel column chromatography