A coupled system comprising a photoreactor combined with a sequential batch bioreactor (SBR) was evaluated for the degradation of a Cibacron Yellow LS-R commercial dye. The photoreactor was evaluated by comparing synthesized 0.1% Fedoped TiO2 with titanium dioxide P-25. The photoreactor demonstrated satisfactory performance in color and DOC removal of 94.5% and 37.6%, respectively. These results were only slightly inferior to those obtained using the commercially available catalyst TiO2 P-25 over six hours of operation. The photoreactor increased the dye biodegradability from 0.1 to 0.47 over four hours of phototreatment with the synthesized 0.1% Fe-doped TiO2 photocatalyst. The coupled system completed the dye degradation in 34 hours, reaching a mineralization level of 70%, measured as COD. These results are remarkable, considering that the biological process as a single treatment did not lead to dye removal.