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With pyridine; potassium permanganate; water; at 100.0℃; for 4.0h;
To a solution of 2-chloro-3-fluoro-5-methylpyridine (512 mg, 3.S2mmol) in pyridine (2.5 mL) and water (2.5 mL) was added one portion of potassium permanganate (1.1 g, 6.9 mmol). The reaction mixture was heated to 100 C. Two more equal portion of potassium permanganate (for a total of 3.3 g, 20.7 mmol) were added afterrespectively 1 h and 2 h of stirring at 100 C. When needed, the solid accumulated in the condenser were washed down with water and pyridine. After another 1 h of stirring at 100 C, the reaction mixture was cooled down to room temperature. The reaction mixture was quenched with saturated aqueous Na2S2O3 and stirred 30 minutes. The mixture was filtered, then acidified to pH 2 with HC1 5 M. The aqueous layer was extracted with EtOAc (3x). The combined organics were washed with brine (lx), dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by silica gel flash chromatography eluting with 90% to 70% PE-EtOAc gradient to give the title compound as a white solid (300 mg, 49%).
With pyridine; potassium permanganate; water; at 100.0℃; for 4.0h;
b) -Chloro-S-fluoronicotinic acidPotassium permanganate (1.09 g, 6.87 mmol) was added to a mixture of 2-chloro-3-fluoro- 5-methylpyridine (0.5 g, 3.43 mmol), water (2 mL) and pyridine (2 mL) and the mixture was heated at 100 0C for 1 h. Solid material stuck in the reflux condenser was washed down with pyridine. More potassium permanganate (2.17 g, 13.7 mmol) was added in portions and heating at 100 0C was continued for a total of 3 h. The reaction mixture was filtered to remove the solids and the filtrate was concentrated to give the crude title compound. MS (ESI) m/z 174 [M-I]".
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