Production of the distilled alcohol pisco results in vinasse, dark brown wastewater with high polyphenols contents and chemical oxygen demand (COD). No prior research exists on the efficiency of advanced oxidations processes (AOPs) in treating pisco vinasse. Therefore, the purpose of this study was to assess the efficiency of ultraviolet (UV), ultrasound (US), US + UV, heterogeneous photocatalysis (HP), and HP + US treatments. Polyphenols, COD, and color removal, as well as oxidation-reduction potential, were monitored over a 60-minute treatment period. Energy consumption levels and synergies were also calculated. The HP + US treatment achieved the best removal ratios for polyphenols (68%), COD (70%), and color (48%). While the HP treatment was the second most efficient in terms of polyphenols (62%), COD (58%), and color (40%) removal, this AOP comparatively required the least amount of energy. Considering the energy efficiency and relatively high pollutant-removal rates of the HP treatment, this AOP is recommended as a practical alternative for treating pisco vinasse.