Ammonium hexachloroplatinate (NH 4) 2 PtCl 6, owing to its low solubility in NH 4 Cl containing aqueous solutions, is an intermediate compound during the hydrometallurgical extraction of platinum. As a rare example of a water soluble and air stable platinum(IV) salt that is not hygroscopic, (NH 4) 2 PtCl 6, may be a convenient and economic platinum precursor for large-scale catalyst production. This report investigates the feasibility of (NH 4) 2 PtCl 6 as Pt precursor for synthesis of the electrocatalysts for polymer electrolyte membrane fuel cells (PEMFCs), i.e., the Pt supported on high surface area carbon (Pt/C). The Pt/C electrocatalysts with ~20 wt.% Pt loading are synthesized through a microwave assisted polyol synthesis approach. The reaction parameters, namely the reaction time and the reaction temperature are optimized. In terms of the electrochemical surface area, Pt/C electrocatalyst synthesized at a reaction temperature of 140 o C and a reaction time of 150 s using a Pt concentration of 5 mM exhibited the optimal performance. The process may be used to synthesize