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Diethyl 1-(<i>N</i>-acetylamino)-1-(diphenylphosphinoyl)-1-phenylmethylphosphonate was synthesized at room temperature, starting from 1-ethoxy derivative of diethyl 1-(<i>N</i>-acetylamino)-1-phenylmethylphosphonate via the corresponding phosphonium salt as a reactive intermediate in the Michaelis–Arbuzov-like reaction with methyl diphenylphosphinite. The structure of the compound obtained was confirmed by spectroscopic techniques (¹H, ¹³C, ³¹P NMR, IR, and MS).