Integrating MOFs as precursor, especially for employing N-containing organic linkers, with sulfides is an effective method to prepare the highly efficient N-doped carbon supported metal-based catalysts for hydrogenation of nitroarenes. In this work, a N,Fe-containing metal organic frameworks (MOFs; termed as MIL88-HMTA) with spindle-like structure was prepared via self-assembly method, in which hexamethylenetetramine (HMTA) linker was introduced as N source. Subsequently, N-doped carbon supported FeS x -Fe 2 O 3 catalyst (named FeS x -Fe 2 O 3 @CN) was fabricated upon the pyrolysis of sulfurized MIL88-HMTA. Catalytic experiments reveal that the FeS x -Fe 2 O 3 @CN delivered excellent performance for hydrogenation of nitroarenes in comparison with those of catalyst without sulfidation process (Fe 2 O 3 @CN) and conventional MIL88 derived catalyst (Fe 2 O 3 @C). The XRD, TEM, SEM/EDX, Raman, UV, and XPS analyses have revealed that the developed FeS x -Fe 2 O 3 @CN catalyst exhibited outstanding catalytic efficiency was ascribed to synergistic effect between FeS x and Fe 2 O 3 species, abundant structural defects, more Fe-N x species, and strengthened decomposition ability of hydrazine hydrate (N 2 H 4 ÁH 2 O). Furthermore, the effect of sulfidation ratio (the mass ratio between thioacetamide and MIL88-HMTA) towards preparation of the developed FeS x -Fe 2 O 3 @CN on the catalytic activity of hydrogenation reaction was also systematically performed. Notably, the optimized catalyst (denoted as FeS x -Fe 2 O 3 @CN-8) exhibited unexpected performance and recyclability for hydrogenation of nitroarenes under mild condition. The pyrolysis of sulfurized N-containing MOFs may present a facile approach for fabricating MOFsderived N-doped carbon supported catalysts, which provides a potential application in heterogeneous catalytic reactions.