Poly(methylphenylene) (PMeP) films were prepared by direct oxidation of toluene in the mixed electrolytes of boron trifluoride diethyl etherate (BFEE) and trifluoroacetic acid (TFA). The oxidation potential of toluene in pure BFEE was measured to be 1.52 V versus saturated calomel electrode (SCE). This value was much lower than that determined in a neutral medium such as acetonitrile (2.13 V versus SCE). The introduction of TFA into BFEE decreased the oxidation potential of toluene and also improved the properties of as-formed polymer films. Infrared and Raman spectra confirmed the formation of PMeP films. (C) 2004 Wiley Periodicals, Inc.