In this study, [(N-benzamidomethyl)(N-benzoyl)amino]methyltriphenylphosphonium tetrafluoroborate was synthesized at 80 °C, starting from N-benzoylaminomethyltriphenylphosphonium tetrafluoroborate, by a specific α-amidoalkylation reaction using Hünig’s base as a catalyst. N-benzoylaminomethyltriphenylphosphonium tetrafluoroborate acts as both an amidoalkylating agent and a nucleophile precursor. The structure of the compound obtained was confirmed by spectroscopic methods (1H-, 13C-, 31P-NMR, IR) and HR-MS analysis.