Nitric Acid → 2-Chloro-4-fluoro-5-nitrobenzoic Acid

Participants

Reaction Steps

A blend of 70% nitric acid (64.5 gm) and concentrated sulfuric acid (65 mL) was added dropwise over an hour period to a suspension of 2-chloro-4-fluoro-benzoic acid (125.0 gm, 716 mL). The white suspension was stirred mechanically for 30 minutes at ambient temperature. The thick white suspension was carefully poured into ice-water (100 mL). Ethyl acetate (800 mL) was added. The organic layer was separated, dried (MgSO4) and evaporated to dryness under vacuum to give the title compound of Step A as a white solid (156.0 gm, 99%); m.p. 134°-136° C.; IR (cm-1), C=O (1719.8). This intermediate was used without further purification.

Provenance & Evidence