A new well‐defined telechelic macrophotoinitiator of polystyrene was synthesized by combination of ATRP and click chemistry. The ATRP of styrene by means of 2‐oxo‐1,2‐diphenylethyl‐2‐bromopropanoate (PI‐Br) initiator with CuBr/2,2′‐bipyridine yields polystyrene with photoactive benzoin (PI) and bromine (Br) group (PI‐PSt‐Br). Subsequently, PI‐PSt‐Br was converted to PI‐PSt‐N3 by simple nucleophilic substitution reaction. Alkyne functionalized benzoin (PI‐alkyne) was synthesized by using benzoin photoinitiator and propargyl bromide. Then the coupling reaction between PI‐PSt‐N3 and PI‐alkyne was performed by Cu(I) catalysis. The spectroscopic studies revealed that low‐polydispersity polystyrene with desired photoinitiator functionality at both end of the chain, PI‐PSt‐PI, was obtained.

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