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This study synthesized the metal–organic framework-derived composite Fe–N–Co@C-800-acid-leaching (Fe–N–Co@C-800-AL) through co-doped iron and nitrogen atoms in a zeolitic imidazolate framework-67, followed by pyrolysis at 800 °C and the AL process. Fe–N–Co@C-800-AL was highly active in an oxygen reduction reaction, during which the number of transferred electrons (3.986) was close to an ideal four-electron transfer. In addition, Fe–N–Co@C-800-AL showed no obvious degradation, even after potential cycling of half-cell measurement (30 000 cycles). The prepared material exhibited a porous structure composed of nanoparticles (NPs) that were randomly distributed on poly-hydrocarbon structures with a Brunauer–Emmett–Teller surface area of 449.0 m2 g–1. X-ray photoelectron spectroscopy demonstrated that the synthesized Fe–N–Co@C-800-AL contained large amounts of pyridinic nitrogen and graphitic nitrogen, which could significantly enhance the activity of the oxygen reduction reaction. Furthermore, X-ray absorption spectroscopy of Fe−N−Co@C-800-AL revealed the existence of Co–Co and Fe–Fe and a lack of Co–N x and Fe–N x moieties, which means an oxygen reduction reaction may occur on the microstructures of N-doped carbon with wrapped metal NPs (Co or Fe). These findings revealed that Fe–N–Co@C-800-AL had a porous structure, high surface area, and the presence of functional nitrogen, thereby making it suitable for oxygen reduction reaction.