反应详情

温度

50 °C

To a stirring solution of 243 mg (1.6 mmol) of methyl 5-aminonicotinate in 5 mL of HF-pyridine at 0° C. was added 119 mg (1.72 mmol) of NaNO2. The mixture was stirred at 0° C. for 30 min. and at 50° C. for 1 h. The reaction was quenched by ice and sat. NaHCO3 solution. The aqueous layer was extracted with CHCl3, dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (1% MeOH/CHCl3) provided 139 mg of methyl 5-fluoronicotinate as a yellow solid in 56% yield.

1. customThe reaction was quenched by ice and sat. NaHCO3 solution
2. extractionThe aqueous layer was extracted with CHCl3
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification by flash silica gel chromatography (1% MeOH/CHCl3)