The preparation of thermally stable fluoropolymers was investigated using three approaches, each based on the synthesis of a different type of fluorocarbon alkoxide monomer. Two of these alkoxides were prepared by the reaction of potassium fluoride with bisfluorosulfonate COMPOUNDS. One alkoxide is extremely stable, whereas the other is formed only as a transient intermediate. Neither polymerized with perfluorocyclobutene. A prototype of the third type of monomer was prepared, but it too failed to react with perfluorocyclobutene. Results indicate that the reactivity of perfluorinated alkoxides is extremely sensitive to structure.