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Block copolymers with tunable compositions offer theability todirectly control the interaction strength between the two blocks andtherefore polymer properties. The miscibility of an A–B blockcopolymer can be increased by introducing B or B-like comonomers intothe A block, and literature has shown that both the amount and thedistribution of these comonomers affect the compatibility of the twoblocks. Sequence-defined block copolymers in which one can exactlycontrol the composition and comonomer distribution provide a uniqueopportunity to control the overall strength of segregation. Here,sequence-defined block copolymers have been synthesized via azide–alkynecoupling using polystyrene and sequence-specific polypeptoids (N-substitutedglycines) with 2-methoxyethyl side chains. These polystyrene-polypeptoidblock copolymers readily self-assemble into hexagonally packed andlamellar morphologies. N-(2-phenylethyl)glycine residues,which have a styrene-like side chain, were introduced throughout thepolypeptoid block to increase the compatibility with the polystyreneblock. As the compatibility increased, the strength of segregationand therefore the block copolymer order–disorder transitionsdecreased. The polystyrene–polypeptoid block copolymers providea tunable platform for further studies on the effect of compositionand sequence design on self-assembly and block copolymer properties. [ABSTRACT FROM AUTHOR]