PtRh nanoparticles were successfully synthesized by one-step chemical strategy, consisting in the thermolysis of a suitable Pt and Rh precursors in organic solvent in the presence of surfactants. This way provides experimental easiness and potential low-cost production. Transmission electron microscopy – Energy dispersive X-ray spectroscopy (TEM-EDS), thermogravimetric analysis coupled with mass spectromery (TG-DTG-MS) and X-ray diffraction (XRD) were employed for characterization. The nanoparticles showed an average diameter of about 1–3 nm. The result of the EDS analysis confirmed a Pt/Rh atomic ratio in line with the percentages of Pt and Rh in the precursors chosen for the synthesis. The facile synthesis of amidyl radicals used in intramolecular hydroaminations to produce isoindolinones, using a PtRh cathode in a flow system was demonstrated.