Several derivatives of higher homologues of bis-fused TTF, BDT-TTPY (1) and DT-TTP (2), have been synthesized. Cyclic voltammograms of 1 and 2 consist of three-pairs of double-electron and five-pairs of single electron redox waves, respectively. Most of cation radical salts obtained by the chemical doping with appropriate oxidants showed relatively high conductivity (sigma(rt) = 10(-2)-10(1) S cm(-1) on compressed pellets).