A new methodology for the synthesis of azachalcones has been developed to avoid formation of secondary products of dimerization and cyclization, based on the rigorous control of the pH of the reaction medium. The method was applied to obtain 4 substituted azachalcones, which were condensed with 4-ciclohexiletiosemicarbazide. The tridentate ligands containing derived from 2-acetilpyridine thiosemicarbazones were synthesized and characterized by 1HRMN, 13C-NMR, FTIR spectroscopy. On the basis of the ligand and copper salt was obtained a coordination compound, which will be tested on its biological activity.