Acetic Anhydride → HCID 18629343, compound

Participants

Reaction Conditions

Reaction Steps

744 ml of acetic anhydride was added to 77.97 g of 4-chloro-3-difloromethoxy-2-methylpyridine N-oxide (VI), which was heated at 100° C. for 4 hour. The solvent was distilled off under reduced pressure and 2N sodium hydroxide was added thereto to adjust to pH 11 and the resulting mixture was heated at 100° C. for 1 hour. The resulting mixture was extracted with chloroform and the resulting organic layer was washed with saturated salt water and dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; chloroform:ethyl acetate=5:1) to obtain 23.11 g of 4-chloro-3-difluoromethoxy-2-hydroxymethylpyridine (VII).

Provenance & Evidence