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A macrocyclic hydrazone Schiff bases were synthesized by reaction of pyridine-2,6-dicarbohydrazide and pyridine-2,6-thiodicarbohydrazide with dicarbonyls. Schiff bases have been characterized by melting point, elemental analyses, LC-MS, IR, 1 H and 13 C NMR spectral data. The Schiff base from pyridine-2,6-dicarbohydrazide and benzil has been studied by liquid–liquid extraction towards the d-metal ions (Cu(II) and Cr(III)) from aqueous phase to organic phase. The effect of chloroform and dichloromethane as organic solvents over the metal chlorides extraction was investigated at 25 ± 0.1°C by using flame atomic absorption.