Attempts to prepare and isolate α, α, α′, α′-tetrafluoro-p-xylylene (III) from several compounds designed as precursors were not successful. Pyrolysis of α, α, α′, α′- tetrafluoro-p-xylene (V) gave a mixture of β, β, p-trifluorostyrene (XIV) and 1, 1, 5- trifluorobenzocyclobutene (XIX). A novel synethsis of XIV was achieved.