Nitric Acid → HCID 18695462, compound

Participants

Reaction Steps

In 16.ml of concentrated sulfuric acid, 3.29 g (11.8 mmol) of ethyl 4-(2,4-difluorophenoxy)benzoate was dissolved at the temperature not higher than 5° C. To the resulting mixture, 520 pl of fuming nitric acid was added at -5° C. or lower under stirring, followed by stirring for 30 minutes at the same temperature. The reaction mixture was poured into ice water and the insoluble matter so precipitated was collected by filtration. The resulting compound was dissolved in chloroform. The resulting solution was washed successively with water and brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting residue was purified by chromatography on a silica gel column (developing solvent: hexane:ethyl acetate=8:1) to give 2.42 g (63%) of ethyl 4-(2,4-difluoro-5-nitrophenoxy)benzoate.

Provenance & Evidence