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The mechanism of copolymerization of fluoronitrosoalkanes with fluoroolefins was investigated. The reaction was not inhibited by water or other common ionic polymerization inhibitors but was greatly affected by free radicals or radical chain transfer agents, indicating a free radical polymerization mechanism. Evidence against initiation by impurities or by homolytic cleavage of the nitroso monomer was obtained. Initial rates of polymerization in solution were determined. The data obtained is consistent with a polymerization mechanism involving initiation by a radical formed through the interaction of the fluoroolefin with the fluoronitrosoalkane which has a significant diradical or triplet state population at the polymerization temperature. The reactivities of various monomers, the formation of low molecular weight product and the structures of the oxazetidine by‐products are discussed in terms of this mechanism.

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