Herein, we report on a new and innovative post-polymerization modification procedure for the ethylene-free synthesis of polyethylene copolymers and block copolymers. Poly[N-(acryloyloxy)phthalimide] statistical and block copolymers synthesized by straightforward reversible-deactivation radical polymerization are used for thermally and photochemically induced metal-catalyzed decarboxylation yielding polyethylenes by the formation of a secondary radical at the polymer backbone that is able to react with a hydrogen source. The presented route toward various polyethylene structures via decarboxylation reactions establishes a new synthetic method in polymer chemistry, namely, the straightforward and efficient synthesis of different polyethylene block copolymers.

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Herein the decarboxylation of poly[N‐(acryloyloxy)phthalimide] (PAP) for the synthesis of functionalized polymers is reported. PAP homopolymer and block copolymers are used as precursor polymers for the straightforward functionalization via decarboxylation and subsequent Michael‐type addition or nitroxide radical coupling (NRC).

The straightforward electrochemically-initiated radical polymerization of three reactive monomers, i.e. 2,6-difluorophenyl acrylate (DFPA), pentafluorophenyl acrylate (PFPA), and glycidyl methacrylate (GMA), using a simple commercially available electrochemical setup for the generation...

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