Synthesis and reaction chemistry of fluoroxydifluoromethyl fluoroformyl peroxide

The reaction of bis(fluoroformyl) peroxide 1 with F2 in the presence of CsHF2 of KHF2 produces FOCF2OOC(O)F 2 in 60% yield. The previously known FOCF2OOCF2OF is also obtained as a byproduct along with small amounts of the new compounds FOCF2OOC(O)OOC(O)F 3 and FOCF2OOC(O)OOCF2OF 4. Hydrolysis of 2 affords either FOCF2OOC(O)OOCF2OF 4 or FOCF2OOH 5 in low yield, depending on the reaction conditions. Fluorination of peroxides 3–5 provides the corresponding fluoroxy compounds in high yields and provides further proof of structure.