Abstract Low-temperature ozonation of isopropyl alcohol (1 a) and isopropyl methyl ether (1 b) in [D 6] acetone, methyl acetate, and tert-butyl methyl ether at− 78 C produced the corresponding hydrotrioxides, Me 2 C (OH)(OOOH)(2 a) and Me 2 C (OMe)(OOOH)(2 b), along with hydrogen trioxide (HOOOH). All the polyoxides investigated were characterized for the first time by 17 O NMR spectroscopy of highly 17 O-enriched species. The ...