We presented a one‐pot approach to functionalized macroinimer via living free‐radical polymerization. The living free‐radical copolymerization of the mixture of (N,N‐diethyldithiocarbamyl)methyl styrene (DTCS), maleic anhydride (MA), and styrene (100:10 equiv mixture of styrene and MA) was studied in tetrahydrofuran under UV irradiation. The formation of alternating sequences was initially fast with preferential consumption of styrene and MA. Further polymerization involved growth of a homopolystyrene block.
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