Аннотация:A new representative of hybrid pincer ligands has been synthesized by the thiocarbamoylation of a potassium salt of 3-(quinoxalin-2-yl)phenol with ClC(S)NMe2 to probe its cyclopalladation features in solution and under solvent-free conditions. The compound obtained is shown to readily undergo cyclometalation under the action of PdCl2(NCPh)2 upon heating in benzonitrile and, more importantly, in the absence of an added solvent, using the preliminary ground mixture of reactants as the starting material, which provides a powerful and green alternative to the conventional solution-based synthesis. The course and outcome of the solid-phase reaction were analyzed by IR spectroscopy, elemental and SEM/EDS analysis. The possibility to scale up the solid-phase synthesis using a simple thermoreactor was demonstrated for the first time. The resulting palladacycle exhibited high cytotoxic activity against several solid and hematopoietic cancer cell lines.