| Summary: | The reaction of FeCl<sub>3</sub>, SeO<sub>2</sub>, and Pyridine (Py) in the presence of methanol (MeOH) under CO pressure generates a black precipitate, which has been confirmed as ferric di-selenide, FeSe<sub>2 </sub>through different structure characterization methods. Furthermore, impregnation of 5 wt% of FeSe<sub>2</sub> onto γ-Al<sub>2</sub>O<sub>3 </sub>exhibits better catalytic performance than FeSe<sub>2</sub> due to the highly dispersed and smaller particle sizes ca. 200–300 nm. The reductive carbonylation of nitrobenzene (NB) was investigated over FeSe<sub>2</sub>/γ-Al<sub>2</sub>O<sub>3</sub> as a heterogeneous catalyst, delivering an excellent yield and high selectivity of methyl-<i>N</i>-phenyl carbamate (MPC). Moreover, a set of reactions was performed with variation in the reaction time, temperature, and pressure to investigate the effects of these factors. In particular, FeSe<sub>2</sub>/γ-Al<sub>2</sub>O<sub>3</sub> is highly stable and can be recycled for up to five cycles without significant loss in catalytic performance. A mechanistic study was also conducted on this low-cost catalyst system, especially proposing a crucial role of FeSe<sub>2 </sub>(μ-CO) active species.
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