Abstract Reaction of 1, 1, 1-trifluoropropanone (trifluoroacetone)(1a) with 30% hydrogen peroxide in the presence of conc. sulfuric acid afforded in good yield 3, 6-bis (trifluoromethyl)- 3, 6-dimethyl-1, 2, 4, 5-tetroxane or trifluoroacetone diperoxide (2a). Peroxide 2a is quantitatively converted into trifluoroacetone (1a) and dioxygen by a catalytic amount of tetrabutylammonium iodide through a reductive electron transfer chain reaction carried out ...