Abstract N , N ′ -Dipropionitrile acrylamide (DPAAm) monomer was synthesized by the reaction of 3,3 ′ -iminodipropionitrile with acryloyl chloride. This monomer was polymerized by using AIBN as initiator in ethanol solution at 70 °C and a conversion of 77% obtained. The polymer reacts with hydroxylamine to afford a new polymer containing two pendant amidoxime groups in each monomeric unit. The conversion of the nitrile groups to amidoxime group was followed by FT-IR spectroscopy. The structure of poly(DPAAm) and amidoximated poly(DPAAm) were also characterized by proton nuclear magnetic resonance ( 1 H NMR) spectroscopy further confirming amidoximation.