A new aromatic diamine, 2,3-bis(4-(4-amino-2-(trifluoromethyl) phenoxy)phenyl)naphtho[2,3-f]quinoxaline-7,12-dione, was synthesized and fully characterized by using FTIR, 1H and 13C NMR, DEPT technique, and elemental analysis. A series of novel fluorescent anthraquinone-quinoxaline containing polyamides (PAs) with inherent viscosities of 0.39–0.62 dL/g was prepared by direct polycondensation of the diamine with various dicarboxylic acids. These PAs were readily soluble in many polar aprotic organic solvents and could be solution-cast into tough and flexible films. The PAs exhibited glass transition temperatures (Tg)s between 230 and 323 C, and 10% weight loss temperatures in the range of 362–433 C in N2. All of the PAs have fluorescence emission in solution and in solid state with maxima around 452–510 nm and with the quantum yields in the range of 6–17%. Also, cyclic voltammetry (CV) method was used to study the electrochemical oxidation behavior of these polymers at the surface of a modified multiwalled carbon nanotube (MWCNT)s glassy electrode.