A new unsymmetrical tetrathiafulvalenes (TTF) containing nitrophenyl or aminophenyl rings were prepared by using a cross-coupling method of the respective 4,5-dialkyl-1,3-dithiole-2-one 1a-e with 4-(p-nitrophenyl)-1,3- dithiole-2-thione 2. The conversion of the nitro moiety 3a-e to amino groups’ 4a-e used reduction reaction. The reducing power of each new precursor was determined by cyclic voltammetry. Charge transfer complexes of the donors with tetracyanoquino-dimethane (TCNQ) were prepared and characterized. The electrical conductivity of these materials was measured and discussed