| Summary: | A semi-crystalline iron-based metal-organic framework (MOF), in particular Fe-BTC, that contained 20 wt.% Fe, was sustainably synthesized at room temperature and extensively characterized. Fe-BTC nanopowders could be used as an efficient heterogeneous catalyst for the synthesis of dihydroxybenzenes (DHBZ), from phenol with hydrogen peroxide (H<sub>2</sub>O<sub>2</sub>), as oxidant under organic solvent-free conditions. The influence of the reaction temperature, H<sub>2</sub>O<sub>2</sub> concentration and catalyst dose were studied in the hydroxylation performance of phenol and MOF stability. Fe-BTC was active and stable (with negligible Fe leaching) at room conditions. By using intermittent dosing of H<sub>2</sub>O<sub>2</sub>, the catalytic performance resulted in a high DHBZ selectivity (65%) and yield (35%), higher than those obtained for other Fe-based MOFs that typically require reaction temperatures above 70 °C. The long-term experiments in a fixed-bed flow reactor demonstrated good Fe-BTC durability at the above conditions.
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