Mesoporous carbonaceous materials were functionalized with iron or copper by a mechanochemical approach. The structural and textural properties of these catalysts were characterized by N2 physisorption, transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The synthesized materials were evaluated in the transformation reaction of trans-ferulic acid using H2O2 as a green oxidant and acetonitrile as a solvent. Furthermore, all the materials were evaluated during three reaction cycles to study their stability and reusability. Inductively coupled plasma mass spectrometry (ICP-MS) was employed to demonstrate that there was no significant metal leaching in the reaction mixture. A 50% selectivity to vanillin was obtained under optimum conditions (remaining at similar values) after three subsequent reaction cycles of 6 h for a Cu/C catalyst at a 0.5 wt % copper load. ©