Abstract: Benzene, halobenzenes, and a number of more or less deactivated arenes, including nitrobenzene, readily reacted in anhydrous HIO 3/AcOH/Ac 2 O/conc. H 2 SO 4 mixtures to probably give ArIO 2 intermediates or other hypervalent species (not isolated). The final reaction mixtures were poured into excess aq. Na 2 SO 3 solution (a reductant) to give the purified iodinated products in 39-83% yields.