LAUSR

Hydrogenolysis of C−O bonds is a highly challenging reaction with the most efficient catalysts based on bimetallic assemblies. Systematic studies to identify the optimum metal combination have not been performed and, therefore, we designed a method to screen multi‐metallic catalysts, including all water stable transition metals, using diphenyl ether as a model substrate. Bimetallic Pd−Pt (70 : 30) nanoparticles were the most efficient, catalyzing the hydrogenolysis of the C−O bond in diphenyl ether at 95 °C and 1 atm of hydrogen in quantitative yield. This research provides insights into the activity of multi‐metallic catalysts in hydrogenolysis reactions. The catalyst was successfully applied in the reductive fractionation of bio‐mass affording key products in near‐quantitative yields.