Acetamide → HCID 58542717, compound

Participants

Reaction Steps

Under a nitrogen atmosphere, acetamide (4.1 g, 70 mmol) was dissolved in DMF (30 mL). Sodium hydride (content: 50% to 72%, 2.4 g, 60 mmol (the content being regarded as 60%)) was added thereto at 0° C. in three portions. The compound 5-chloro-2,3-difluoropyridine (3.0 g, 20 mmol) was then added dropwise at 0° C., and the mixture was stirred for 3 hours, during which time the temperature was allowed to increase to room temperature. The reaction mixture was cooled to 0° C., a saturated ammonium chloride aqueous solution was added, and after the mixture was warmed to room temperature, extraction was performed with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was suspended in a mixed solvent of heptane and t-butyl methyl ether (15:1), and the suspension was stirred at room temperature. The suspension was filtered, and the obtained solid was dried under reduced pressure to obtain the title compound (2.7 g).

Provenance & Evidence