反应详情

To a solution of 4-methoxy-2-pyridinecarbonitrile (5.35 g, 38.6 mmol) in benzene (50 ml) and ether (50 ml) cooled to 0° C. was added dropwise over 20 min a 2M slution of MeMgI in ether (23 ml, 46.3 mmol). After 0.5 h, the mixture was allowed to warm to ambient temperature, and stirring continued for 2 h. The mixture was cooled to 0° C. and 2M aqueous HCI (100 ml) added. The mixture was made basic with saturated aqueous sodium bicarbonate (˜80 ml) and the organic layer separated and dried (MgSO4). After removal of solvent, the residue was purified by flash chromatography eluting with ethyl acetate/hexane (1:5) to afford 3.60 g (60%) of 2-acetyl-4-methoxypyridine.

1. waitcontinued for 2 h
2. temperatureThe mixture was cooled to 0° C.
3. addition2M aqueous HCI (100 ml) added
4. customthe organic layer separated
5. dry with materialdried (MgSO4)
6. customAfter removal of solvent
7. customthe residue was purified by flash chromatography
8. washeluting with ethyl acetate/hexane (1:5)