This work reflects the synthesis and NMR characterization of a new di-phosphonated ligands, precursor of the VIII group metals (Ir, Rh, Pt, Ru and Pd) complex compounds as potential catalyst for CO2 reduction and H2 production/oxidation. The reaction pathway is an adaptation of a literature method [1, 2], involving the reactions between 2-aminomethyl pyridine with diethyl phosphite in the presence of paraformaldehyde according to Scheme 1. The resulting product was obtained as an orange liquid compounds upon chromatographic separation. The structure of the compounds was confirmed by spectroscopic NMR methods (1H NMR, 13C NMR and 31P NMR as well as COSY, HMQC and HMBC experiments). NNH2(C2H5)2PO3HHO(CH2O)nHNNPO3(C2H5)2PO3(C2H5)2 Scheme 1. Reaction scheme of N-(methylene-2-pyridine)-N,N-bis(diethoxyphosphorylmethyl)amine.