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

Participants

Reaction Conditions

Reaction Steps

1.77 g (10 mol) of 2,3,4-trifluoronitrobenzene are added to 2.5 l of water, and the mixture is warmed to 40° C. and vigorously stirred. 1320 g (22 mol) of 40% strength lithium hydroxide solution are then added dropwise in such a way that the temperature rises from 40° to 55° C. within 2.5 h. After this time, GC checking no longer shows any starting compound. The reaction mixture is brought to pH 2 with 70% strength sulfuric acid. It is then worked up, as described in Examples 1 and 2. 1.48 kg of 2,3-difluoro-6-nitrophenol having a purity >99.9% (GC) are obtained after drying (melting point 63.5° C.), which corresponds to a yield of 85% of theory.

Provenance & Evidence