反应详情

To a solution of 5-bromo-2-methoxy-3-methyl-pyridine (1.0 g, 5.0 mmol) in DMF (10 ml) was added CuCN (0.534 g, 6.0 mmol) and the resulting mixture is heated at reflux for 28 h. After cooling to room temperature the mixture is diluted with EtOAc and washed with 10% ammonia solution followed by water and brine solution. The organic layer was separated, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by flash chromatography (5% EtOAc/Hexane) to give 5-cyano-2-methoxy-3-methyl-pyridine (36) (0.68 g, 93%).

1. temperaturethe resulting mixture is heated
2. temperatureat reflux for 28 h
3. washwashed with 10% ammonia solution
4. customThe organic layer was separated
5. dry with materialdried over MgSO4
6. customevaporated under reduced pressure
7. customThe residue was purified by flash chromatography (5% EtOAc/Hexane)