Abstract: Activated carbon (AC) was successfully synthesized by a chemical activation method using as the source of fronds of Cocus nucifera (C. Nucifera). The formation of fronds of C. Nucifera activated carbon (CNF-AC) and its physicochemical properties were investigated systematically. The morphology, surface area and porosity, of the synthesized materials were investigated using X–ray diffraction studies (XRD), HRSEM, N2 adsorption–desorption (BET) analysis. The excellent catalytic activity of CNF-AC (800 oC) was revealed in the selective oxidation of toluene to the corresponding benzaldehyde with 85% conversion and 87% selectivity. The material was evaluated for the oxidation of toluene in the presence of tert-Butyl hydroperoxide (tBHP) as the oxidizing agent and tetrahydrofuran (THF) solvent. Hence, the obtained results noted that the material was highly active, stable and can be recycled at least four times without a loss of catalytic efficiency. The CNF-AC was carried out in a sealed graphite crucible maintained at a temperature of 800 oC for the transformation of C. Nucifera into porous activated carbon to achieve the excellent catalytic activity.