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The aim of this book is to investigate the versatility of Cu(0)-mediated reversible deactivation radical polymerisation (RDRP) in aqueous media in order to facilitate the synthesis of multiblock copolymers consisting of various acrylamides. Under carefully optimised conditions, a simple and highly efficient one-pot polymerisation procedure (full conversion for each block and no intermediate purification required) will be developed allowing access to iterative monomer additions, fast polymerisation rates and high level of control. As a result, complex microstructures (such as hexablocks) can be achieved in a quantitative manner in a matter of few hours, which consists the fastest synthesis of such material up to date.