反应详情

To concentrated sulfuric acid (23.81 g), cooled to 0° C., under a nitrogen atmosphere, was added concentrated nitric acid (27.5 g) dropwise. 2-Chloro-5-fluorotoluene (9 g) was added dropwise and the reaction was stirred for 2 hours. The reaction was poured into ice and extracted with ethyl acetate. The organic phase was washed with aqueous sodium hydrogen carbonate, dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by silica column chromatography [eluting with ethyl acetate/heptane (1:2)] to yield the title compound (9.4 g).

1. additionThe reaction was poured into ice
2. extractionextracted with ethyl acetate
3. washThe organic phase was washed with aqueous sodium hydrogen carbonate
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica column chromatography [eluting with ethyl acetate/heptane (1:2)]