反应详情

2,5-Difluoro-N-(2-fluoro-3-hydroxymethyl-phenyl)-benzenesulfonamide (75, 950 mg, 2.99 mmol) and stabilized 2-iodoxybenzoic acid (2.608 g, 45%, 4.2 mmol) are dissolved in 150 mL of tetrahydrofuran and the reaction is stirred at room temperature for 16 hours. The reaction is poured into water and extracted with ethyl acetate. The organic layer is washed with brine, dried over sodium sulfate, filtered and the filtrate is concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with ethyl acetate and dichloromethane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (76, 0.944 g). MS (ESI) [M−H+]−=314.

1. extractionextracted with ethyl acetate
2. washThe organic layer is washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationthe filtrate is concentrated under vacuum
6. customThe resulting material is purified by silica gel column chromatography
7. washeluting with ethyl acetate and dichloromethane
8. concentrationconcentrated under vacuum