A short procedure for the preparation of stable arylbipyridylpalladium complexes linked to a polystyrene resin is described. Starting from an o‐iodobenzylalcohol with a pendant azido group, the corresponding supported complex was carbonylated with [13C]CO to produce the desired 13C‐labeled lactone tag with a satisfactory yield of 50%. This 13C‐synthon was obtained with excellent purity after a simple filtration on sintered glass, and further conjugation using CuAAC and SPAAC reactions was performed with model substrates.
13C- and 11C-labelled conjugates were produced in one step upon carbonylation of homogeneous or heterogeneous arylpalladium complexes synthesised by mild C–H activation of gem-dimethylbenzylamine derivatives.
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