In this study, three new aminobiphenylglyoximes, [L 1 H 2 ] N-(2-methoxy)aminobiphenylglyoxime, [L 2 H 2 ] N-(3-methoxy)aminobiphenylglyoxime and L[ 3 H 2 ] N-(4-methoxy)aminobiphenylglyoxime have been synthesized by the reaction of (E,E)-4¢-biphenylchloroglyoxime with 2-Methoxyaniline, 3-Methoxyaniline and 4-Methoxyaniline in absolute ethanol. The preparation Ni II , Co II and Cu II complexes of these ligands are described. The ligands and their complexes were characterized by elemental analyses, IR, mass, H 1 and 13 C NMR spectra, thermogravimetric analyses (t.g.a) and magnetic susceptibility measurements. Ligands complexing properties were studied by the liquid-liquid extraction of selected alkali (Li + , Na + , K + , Cs + ) and transition metals (Co 2+ , Ni 2+ , Cu 2+ , Zn 2+ , Cd 2+ , Pb 2+ ). It has been observed that all ligands show a high affinity to Cu 2+ ions, whereas almost no affinity to alkali metals. The extraction equilibrium constants (K ex ) for complexes of ligands with Cu 2+ metal picrates between dichloromethane and water have been determined at 25°C.