The phosphorus-nitrogen compounds, typically amidophosphoesters/phosphonicamides, are well- known for different applications in flame retardants, and manufacturing of drugs [1–3]. Nuclear magnetic resonance (NMR) is a beneficial technique to study of these compounds, due to the existence of NMR-active nuclei ( 31 P, 1H, 13C). Moreover, NMR spin-spin coupling constants are used to prove the assignment of signals, and analysis related to conformation/configuration [4]. In this work, the synthesis and spectroscopic characterization of two new phosphorus compounds, belonging to diamidophosphoester and phosphonicamide families are investigated. These compounds are (2-Cl-C 6H 4O)(2-Cl-C6 H 4 CH 2NH) 2P(O) (Scheme 1), and (C6H 5)(4-CH 3- C6 H 4 NH) 2 P(O) (Scheme 2). Some topics related to the phosphorus-hydrogen and phosphorus-carbon coupling constants were issued.

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