In this paper, the application of new substituted 2,6-bis((benzoyl-R)amino)pyridine (R = H, 4-Me, and 4-NMe2) derivatives for the recovery of copper(II), nickel(II), cobalt(II), and zinc(II) ions from aqueous solutions was described. The structures of the synthesized compounds were confirmed by nuclear magnetic resonance spectroscopy (NMR), electrospray ionization high-resolution mass spectrometry (ESI HRMS), and tandem mass spectrometry methods (HCD MS/MS). Three different derivatives of 2,6-bis((benzoyl-R)amino)pyridine were used as carriers in membrane processes and as extractants in classic solvent extraction. In each case, the single derivative recovery was carried out on a model solution that contained only one type of metal ions. Spectrophotometry studies were performed to determine the stability constants of the complexes formed by the synthesized species with analyzed metals ions. The results obtained indicate that the synthesized compounds form stable complexes with Cu(II), Ni(II), Co(II), and Zn(II) ions and can be used in both types of studied recovery processes. However, the effectiveness of the synthesized compounds in the recovery of metal ions depends both on the structure of compounds and properties of metals as well as on their concentration.