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A series of phosphonodipeptides containing C\u2010terminal <jats:italic>\u03b1<\/jats:italic>\u2010aminoalkylphosphonic acids was synthesized in satisfactory to good yields conveniently from 2\u2010(<jats:italic>N<\/jats:italic>\u2010benzyloxycarbonylamino)alkanamides, aldehydes, and phosphorus trichloride via Mannich\u2010type reaction and subsequent sequential hydrolysis. The reaction mechanism was proposed and verified by <jats:sup>31<\/jats:sup>P NMR tracing experiments. The current method is an efficient and convenient method for preparation of phosphonopeptides containing C\u2010terminal <jats:italic>\u03b1<\/jats:italic>\u2010aminoalkylphosphonic acids. 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