m-Chloroperbenzoic acid → HCID 13688051, compound

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Reaction Steps

50 g (0.3 mol) of 4-chloro-3-cyano-2,6-dimethylpyridine were dissolved in 1 L of dichloromethane and, at room temperature, 130 g (0.6 mol) of 80% pure m-chloroperoxybenzoic acid were added in portions, and the mixture was stirred overnight and the precipitated m-chlorobenzoic acid was filtered off. Water was added to the filtrate, the pH was adjusted to 12 with solid potassium hydroxide, and the two phases were shaken together to extract. The dichloromethane phase was separated off, dried over sodium sulfate, filtered and evaporated. 4-Chloro-3-cyano-2,6dimethylpyridine 1-oxide was obtained as a solid compound which sintered at 140° C. Yield: 49.3 g (90% of theory).

Provenance & Evidence