This work reports a 1 mol scale catalytic process to synthesize adipic acid directly from cyclohexane in solvent‐free conditions using air as oxidant. Catalysts based on vanadium phosphorus oxides were prepared, characterized and tested. They showed good activity and remarkably high selectivity to adipic acid in comparison to other already known heterogeneous catalysts. The use of solvent‐free conditions permits the easy separation of the product from the reactant mixture, which is very important from the industrial point of view. The process can be used at industrial scale for sustainable adipic acid synthesis. Getting greener with a new one‐pot sustainable and scalable synthesis of adipic acid via solvent‐free air oxidation of cyclohexane.