A new and useful poly(ethylene oxide)-based pH-sensitive block copolymer is introduced. Poly(ethylene oxide-b-N-phenylmaleimide) was first synthesized by anionic polymerization of N-phenylmaleimide (N-PMI) using mixed alkali metal polymeric alkoxide by sequential monomer addition method in the mixture of benzene/THF/DMSO (10/5/3, v/v/v) at room temperature. Reductive deimidation of the resulting block copolymer was performed using hydrazine monohydrate leading to the formation of the corresponding pH-sensitive poly(ethylene oxide-b-maleic acid).