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To a solution of 2-amino-5-fluoropyridine (10 g) in ethanol (200 mL), a solution of chloroacetaldehyde 50percent in water (56 mL, 4.0 equiv.) was added. The reaction mixture was heated at reflux 2 Hrs, then was concentrated under reduced pressure to 100 mL. The residue was diluted in AcOEt (100 mL) and washed with a saturated aqueous solution of NaHCO3 (2* 150 mL). The combined aqueous were saturated with NaHCO3 and extracted back with AcOEt (2*100 mL). The combined organic layers were washed with brine (100 mL), dried over Na2SO4 and concentrated under reduced pressure. Purification by flash-chromatography (MeOH 2.5percent in CH2Cl2) afforded the product as a cream solid (8.7 g, 72percent). M/Z (M+H)+ = 137.
<strong>[109466-87-7]2-Nitro-4-(trifluoromethyl)benzaldehyde</strong> (219 mg) was dissolved in toluene (4 ml), and thereto was added 2-amino-5-fluoropyridine (123 mg), and the mixture solution was refluxed under heating. After the solution was stirred for 3 h, it was kept standing to cool to room temperature, and the solvent was distilled off in vacuo. To the residue was added triethyl phosphite (3 ml), and the residue was heated to 150 C. After the residue was stirred for 4 h, it was kept standing to cool to room temperature, and the residue was purified by the silica gel column chromatography affording the crude product of the compound 2. To the crude product was added hexane (2 ml), and the precipitated material was collected by filtration as the compound 2 (116 mg).MS m/z 282 [M+H]+, APCI(+)
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