Abstract: A convenient preparation of trifluoromethyl hydroperoxide, CF300H, is described and its physical and chemical properties are reported. Trifluoromethyl hydroperoxide behaves as a weak protic acid and readily forms trifluoromethyl peroxides with a variety of reactants. With acid fluorides trifluoromethylperoxy esters are formed in high yield. The synthesis and properties of the new compounds CFsC (0) OOCF3, CH3C (0) OOCF8, CF~ ...