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The radical copolymerization of poly(ethylene glycol maleate) with acrylamide was performed for the fi rst time to obtain 3D cross-linked polymers. The infl uence of temperature, pH of the medium, and organic solvents on the behavior of the synthesized copolymers was studied. The possibility of obtaining nickel nanoparticles in the bulk of the polymer gel for pyridine hydrogenation was demonstrated.Active progress of basic research in the fi eld of radical copolymerization, allowing control of the properties, structure, and molecular mass of the copolymers and the reaction rate, makes it topical to search for new monomers for preparing polymers with a wide spectrum of valuable properties.Unsaturated polyester resins are of much interest from this viewpoint. They readily copolymerize with vinyl monomers. Copolymerization of unsaturated polyester resins was considered for the fi rst time by Boenig [1].The capability of polyester resins to copolymerize with vinyl monomers, e.g., with styrene, was discovered in the middle of the XX century [2].Unsaturated polyester resins based on maleates and fumarates, cured with vinyl monomers, exhibit specifi c physicochemical and physicomechanical properties [1][2][3][4]. Therefore, the production of decorative fi nishing materials and structural items from polyester-styrene copolymers is being actively developed today.Copolymerization of unsaturated polyester resins with acrylates has been studied previously [5][6][7], but data on the related reactions with acrylamide are lacking.The latest studies on copolymerization of unsaturated polyester resins were published in the 1980s. They mainly deal with the development of new formulations for preparing structural materials based on styrene and acrylates. On the other hand, 3D cross-linked copolymers based on unsaturated polyester resins can be highly effective polymeric supports for nanocatalysts based on transition metals. Such compounds are stable and prevent metal particles from aggregation and oxidation for a long time [8].Here we report on a first study of the radical copolymerization of poly(ethylene glycol maleate) with acrylamide in solution to obtain 3D cross-linked polymers and consider the possibility of using these polymers as matrices for preparing catalysts based on nickel nanoparticles. EXPERIMENTALPoly(ethylene glycol maleate) (p-EGM) was prepared by polycondensation of maleic anhydride with ethylene glycol according to the standard procedure [9]. The reaction progress was monitored by determining the acid number and the volume of the released water.The molecular mass (MM) of p-EGM (2350 amu on the average) was determined by the methods of light scattering with a 2100 AN nephelometer (NACH) and of gel permeation chromatography with an Agilent 1260 Infi nity device.