Bis(N-Alkyl-N-diphenylphosphinylmethyl)diglycolamides [Ph2P(O)CH2N(R)C(O)CH2]2O, where R = Et, i-Pr, n-Bu, i-Bu, n-Oct, were synthesized by reaction of diglycolyl chloride with N-alkyl-N-(diphenylphosphinylmethyl)amines Ph2P(O)CH2NHR obtained by the Kabachnik–Fields reaction of aminomethylation of diphenylphosphinous acid, and their hydrochlorides. The structure of the obtained compounds was studied by 1H, 13C and 31P NMR spectroscopy.