Municipal wastewater of Fez city (Morocco) is considered one of contamination sources of the Sebou River in Morocco [1,2]. The present study deals with the fate of phenol as a compound of emergent concerns (CECs) supposed to be persistent after secondary treatment by the conventional processes in wastewater treatment plants (WWTP). Raw wastewater sampling upstream WWTP was performed periodically, followed by an exhaustive characterization. A primary treatment using coagulation-precipitation using ferric chloride was carried out to reduce the initial organic matter load and turbidity. Different treatment factors were optimized using response surface methodology (RSM). Thereafter, the pretreated and simulated wastewaters were spiked with phenol as probe compound, and its degradation was carried out in the heterogeneous Fenton process using synthesized magnetite-supported clay material by the co-precipitation method [3]. Results obtained from wastewater characterization confirm the moderate to high contamination strength of sampled wastewaters, and the preliminary treatment has reduced over 60 % of organics load. Matrix characterization of the pretreated wastewater before coupling to the Fenton process was detailed. On the other hand, the presence of magnetite phase and its high dispersion upon natural clay was confirmed by X-ray photoelectron microscopy (XPS), X-ray diffraction (XRD), and Scanning Electron Microscopy (SEM). Nitrogen adsorption-desorption and Brunauer-Emmett-Teller (BET) measurements showed an optimum clay to magnetite ratio of 2:1 (wt%). The application of heterogeneous Fenton for phenol degradation has been conducted upon simulated and pretreated wastewaters. Results showed almost total degradation of the initial phenol concentration of 50 mg.L-1 within 180 min at pH 3, and the catalyst was reused for several runs. Therefore, coagulation-precipitation coupled to heterogeneous Fenton may be a promising scheme for wastewater treatment.