A new reactive N-substituted maleimide monomer containing an aldehyde function, N-(4-formyl-phenoxy-4′-carbonylphenyl) maleimide (MI-CHO), was synthesized. The radical copolymerization of MI-CHO with styrene was performed at 60 °C in the presence of 2,2′-azoisobutyronitrile as an initiator in dimethylsulfoxide. The copolymerization of MI-CHO with styrene yielded the ‘nearly equimolar’ alternating copolymers for the mole fractions of MI-CHO in the feed ranging from 0.2 to 0.7. The monomer reactivity ratios ( r 1 , r 2 ) in the polymerization of MI-CHO ( M 1 ) with styrene ( M 2 ) and the Alfrey–Price Q 1 and e 1 parameters were determined. The thermal properties of the copolymers were investigated by using thermogravimetric analysis and differential scanning calorimetry.