反应详情

A 2 M solution of 4-fluorophenyl magnesium chloride (7 ml, 14 mmol) was slowly added at −30° C. to a solution of 6-fluoronicotinoyl chloride (3.35 g, 21 mmol,) in ether (30 ml). After complete addition, the cooling bath was removed and the reaction was allowed to reach 10° C. Hydrolysis was performed by addition of water, and the mixture is then diluted with ether. After separation of the layers, the ether solution was washed with brine, dried over Na2SO4 and evaporated in vacuum to yield a yellow solid. After purification by chromatography on silica gel (CH2Cl2/Hexane 85/15), the (4-fluorophenyl)(6-fluoro-3-pyridinyl)methanone 38 was obtained as a white solid (1.52 g, 50%).

1. additionAfter complete addition
2. customthe cooling bath was removed
3. customto reach 10° C
4. customHydrolysis
5. customAfter separation of the layers
6. washthe ether solution was washed with brine
7. dry with materialdried over Na2SO4
8. customevaporated in vacuum
9. customto yield a yellow solid
10. customAfter purification by chromatography on silica gel (CH2Cl2/Hexane 85/15)