A facile synthetic strategy for well‐defined poly(ethyleneimine)‐polystyrene (PEI‐PS) block copolymers utilizing controlled radical polymerization through the macroinitiator approach is presented. Poly(2‐methyl‐2‐oxazoline) containing an alkoxyamine initiating unit at the chain end was prepared by ring opening cationic polymerization of 2‐methyl‐2‐oxazoline through a nitroxide containing initiator. Polymerization of styrene with the poly(2‐methyl‐2‐oxazoline) macroinitiator was carried out under nitroxide‐mediated radical polymerization (NMRP) conditions. GPC and NMR revealed that the polymerization was accurately controlled and well‐defined polystyrene chains were attached to the chain end of the macroinitiator to give the poly(2‐methyl‐2‐oxazoline‐b‐styrene) block copolymers. Hydrolysis of the poly(2‐methyl‐2‐oxazoline) block resulted effectively in poly(ethyleneimine‐b‐styrene) block copolymers.
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