Phosphorus oxychloride → 2,6-Dichloro-4-methylpyridine

関与物質

反応手順

A mixture of 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 7.0 mmol) and phosphorus oxychloride (10 mL) was heated at reflux for 4 h. The volatiles were evaporated and the residue dissolved in ethyl acetate. The solution was washed with ice-water followed by sodium bicarbonate solution. The organic phase was again washed with water, brine solution, dried over anhydrous sodium sulfate and concentrated to obtain a residue which was purified by column chromatography over silica gel (60-120 mesh) using petroleum ether as eluent to afford 2,6-dichloro-4-methyl-pyridine (491 mg, 43%) as a white solid.

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