A zo dyes which are characterized by the presence of the azo chromophore [-N=N-] have attracted much attention not only for their easy preparation and lower cost but also for their wide application in industry as textile dyeing [1][2][3], coloring of plastic and polimers [1,4], colorimetric indicators [5][6], high-technology applications [3,7], cosmetics [8] and photostorage units [4,9]. In addition azo dyes and its derivatives exhibit photoactive properties with potential application as lasers [9] With the advancement in technology, one of the most important scientific problems is how to correlate between chemical and physical properties of the compound [2,15]. The density functional theory (DFT) method is widely used for structural determination of organic compounds, determining the mechanisms of chemical reactions, calculation of the ground state geometries and prediction of spectroscopic data such as UV-Vis, IR and NMR peaks [2,16].In this study we have synthesized new azoazomethine dyes containing acryloyl groups and the compounds were characterized by Uv-Vis, IR and NMR spectroscopy. Also in this research we report the results of DFT calculations to investigate UV-Vis absorption spectrum and FT-IR regions as well as HOMO-LUMO orbital energies, electostatic potential (ESP) maps, chemical hardness and electronegativity of the compounds. Theoretical UV-Vis calculations were carried out in EtOH (polar protic), CH 2 Cl 2 (apolar aprotic) and DMF (polar aprotic) phases in accordance with the phenyl-2-propenoat were synthesized. The acryloyl derivatives of the azo-azomethine dyes were prepared with metallic sodium and acryloyl chloride in 1:1 Molar ratio and characterized using elemental analysis, IR, UV-Vis, 1H-NMR and 13C-NMR spectroscopy. The molecular geometry was also optimized using density functional theory (DFT/B3LYP) method with the 6-311G(2d,2p) and cc-pvtz basis sets in ground state. From the optimized geometry of the compounds, vibrational frequencies, UV-Vis, molecular electrostatic potential distribution and frontier molecular orbitals were performed using same method and basis stets, and the results were compared with the experimental data.