Abstract Four phenylacetylenes (2-R 2 5-R 5-C 6 H 3 C≡ CH: 1a R 2= R 5= CF 3; 1b R 2= CF 3, R 5= CH 3 1c R 2= CH 3, R 5= CF 3; 1d R 2= R 5= CH 3) were synthesized via lithio compounds or Grignard reagent. Bromo-(methyl) benzotrifluorides, the precursors for the lithio compounds, were prepared by the fluorination of the corresponding benzoic with sulfur tetrafluoride. Polymerization using transition metal catalysts provided polyacetylenes in ...