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0 °C

4-Fluoro-1-methylsulfonyl-2-nitrobenzene can be obtained in the following way: 1.3 g of 4-fluoro-1-methylsulfinyl-2-nitrobenzene in 15 ml of dichloromethane are added dropwise to a suspension, stirred at a temperature in the region of −5° C. under argon, of 1.5 g of 3-chloroperoxybenzoic acid in 15 ml of dichloromethane. The reaction mixture is then stirred at a temperature in the region of 0° C. for 30 minutes and is then left to reheat to a temperature in the region of 20° C. It is then filtered through sintered glass and the solid is washed with dichloromethane. The filtrate is washed with an aqueous sodium hydrogencarbonate solution then with water, dried over magnesium sulfate, treated with 3S black, filtered and then concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. The residue thus obtained is purified by chromatography on a column of 125 g of silica (particle size 40-63 μm), eluting with pure dichloromethane. The fractions containing the expected product are pooled and concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. 1.2 g of 4-fluoro-1-methylsulfonyl-2-nitrobenzene are thus obtained in the form of a yellow foam (Rf=0.43, silica gel thin layer chromatography, eluent: dichloromethane)).

1. waitis then left
2. customto reheat to a temperature in the region of 20° C
3. filtrationIt is then filtered through sintered glass
4. washthe solid is washed with dichloromethane
5. washThe filtrate is washed with an aqueous sodium hydrogencarbonate solution
6. dry with materialwith water, dried over magnesium sulfate
7. additiontreated with 3S black
8. filtrationfiltered
9. concentrationconcentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C
10. customThe residue thus obtained
11. customis purified by chromatography on a column of 125 g of silica (particle size 40-63 μm)
12. washeluting with pure dichloromethane
13. additionThe fractions containing the expected product
14. concentrationconcentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C