A versatile new route to zwitterionic diblock copolymers that avoids protecting group chemistry is reported. Various tertiary amine methacrylates are block copolymerized with 2-hydroxyethyl methacrylate to produce hydroxy-functional diblock precursors via sequential monomer addition. These low-polydispersity precursors are then treated with succinic anhydride under mild conditions to produce a range of new near-monodisperse zwitterionic diblock copolymers in which both blocks are weak polyelectrolytes. Thus, the final copolymers exhibit complex aqueous solution behavior (isoelectric points, schizophrenic micellization behavior, etc.) depending on the solution pH.