Sulfuric Acid → 2,3-Difluoro-6-nitrophenol

Participants

Reaction Conditions

Reaction Steps

1.77 kg (10 mol) of 2,3,4-trifluoronitrobenzene are added to 2 l of water, and the mixture is warmed to 40° C. and vigorously stirred. 1760 g (22 mol) of 31.7% strength sodium hydroxide solution are then added dropwise in such a way that the temperature does not rise above 60° C. After about 2 h, GC checking no longer shows any starting compound. The reaction mixture is brought to pH 2.5 using 70% strength sulfuric acid. Steam is then passed into the solution, the product passing over with the steam. The separated solution is cooled to 10° C. with stirring and the precipitated solid is filtered off with suction. The water having a residual content of about 0.1% of 2,3-difluoro-6-nitrophenol can be used in a subsequent batch. 1.48 kg of 2,3-difluoro-6-nitrophenol having a purity >99.9% (GC) are obtained after drying (melting point 64° C.), which corresponds to a yield of 85% of theory.

Provenance & Evidence