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Herein, we fabricated CoCu-0.25-O v with ternary Co...O v ...Cu sites through simple co-precipitation to achieve effective co-utilization of organics and dissolved oxygen (DO) as endogenous electron donor-acceptor in Fenton-like system. Around 100% of dimethylamine (DMA) min within 30 is removed. The involved kinetics (0.22 min−1) and oxidant utilization efficiency (22.5%) are higher than controls with binary sites. Multi-scaled characterizations and theoretical calculations reveal that electron-polarized Co...O v ...Cu sites facilitate co-activation of DMA and DO as electron donor-acceptor through increasing d -band center and lowering work function of catalyst. Meanwhile, ternary sites favor 1O 2 and SO 4 •− generation, and shorten the migration distance of active species to pollutant, thus achieving excellent dual performance improvements. Semi-quantitative results of ESR indicate that DO activation and peroxymonosulfate (PMS) oxidation contribute about three-fourths and one-fourth to 1O 2 production, respectively. This contribution provides a new and sustainable strategy for high-efficiency and oxidant-saving removal of refractory pollutants in the environment. [Display omitted] • Co...O v ...Cu sites greatly improve removal performance of DMA and PMS utilization rate. • Ternary sites activate DMA and DO to replace PMS and favor the formation of ROSs. • Increased d -band center and lower work function of catalyst boost the co-activation. • DMA is removal by enhanced multipath (self-oxidation, 1O 2 and SO 4 •− attacks). • O 2 activation and PMS oxidation contribute 3/4 and 1/4 to 1O 2 formation, respectively. [ABSTRACT FROM AUTHOR]