Abstract 2-Iodoxybenzenesulfonic acid (in a cyclic tautomeric form of 1-hydroxy-1H-1, 2, 3- benziodoxathiole 1, 3, 3-trioxide), a thia-analog of 2-iodoxybenzoic acid (IBX) and a potentially important oxidizing reagent, was prepared by two different pathways: direct oxidation of 2-iodobenzenesulfonic acid and hydrolysis of the methyl ester of 2- iodylbenzenesulfonic acid. The resulting l-hydroxy-1H-1, 2, 3-benziodoxathiole 1, 3, 3- ...