反应详情

To 99 mmol 2-chloro-5-(methylthio) benzoic acid (purchased from Aldrich) in 400 ml methanol at 0° C. was added 296 mmol oxone® and the mixture was allowed to stir at RT for 3.5 h. The precipitate was filtered off and the filtrate was concentrated under reduced pressure. The residue was extracted 3 times with 400 ml ethyl acetate and the combined organic phases washed twice with 300 ml 1 N HCl and with 300 ml saturated aqueous NaCl solution and dried with MgSO4. Evaporation under reduced pressure yielded the title compound which was used in the next step without further purification.

1. filtrationThe precipitate was filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. extractionThe residue was extracted 3 times with 400 ml ethyl acetate
4. washthe combined organic phases washed twice with 300 ml 1 N HCl and with 300 ml saturated aqueous NaCl solution
5. dry with materialdried with MgSO4
6. customEvaporation under reduced pressure