A new radiosynthetic protocol for the preparation of [C-11]aryl nitriles has been developed. This process is based on the direct reaction of in situ prepared L Pd(Ar)X complexes (L = biaryl phosphine) with [C-11]HCN. The strategy is operationally simple, exhibits a remarkably wide substrate scope with short reaction times, and demonstrates superior reactivity compared to previously reported systems. With this procedure, a variety of [C-11]nitrile-containing pharmaceuticals were prepared with high radiochemical efficiency.