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An environmentally friendly and safe synthesis of phloroglucinol and its derivatives through the flow hydrogenation of 1,3,5-trinitrobenzenes on heterogeneous copper catalysts is reported. It was found that hydrogenation of 1,3,5-trinitrobenzene, 2,4,6-trinitrotoluene, 2,4,6-trinitroxylene, and 2,4,6-trinitromesitylene in methanol over Cu–Al mixed oxides derived from layered double hydroxides led to selective formation of the corresponding triaminobenzenes, which were isolated from the reaction mixture in the form of double salts with sulfuric acid and were stable in storage. Subsequent hydrolysis in aqueous solution gave the phloroglucinol derivatives in good yields (75–82%). [ABSTRACT FROM AUTHOR]

Cu-containing layered double hydroxides (LDHs) were synthesized by a co-precipitation method at different reaction conditions, such as aging time, pH, precipitation rate and synthesis temperature. The effect of these parameters on the structure and chemical composition of the catalysts were investigated using a set of physical methods, including thermogravimetric analysis (TGA), X-ray diffraction (XRD), H2-TPR and in situ X-ray photoelectron spectroscopy (XPS). It allowed for checking of the reducibility of the samples. 5-Acetoxymethylfurfural was catalytically hydrogenated to 5-(acetoxymethyl)-2-furanmethanol (AMFM) over Cu-containing catalysts synthesized from layered double hydroxides so as to investigate its catalytic properties in flow reaction. It was shown that synthesis pH decreasing from 10 to 8 resulted in rise of AMF conversion that coincided with the higher surface Cu/Al ratio obtained by XPS. Preferable aging time of LDH materials for obtaining the most active catalyst was 2 h, an amount of time that favored the production of the catalyst with high surface Cu/Al ratio up to 0.38. Under optimized reaction conditions, the AMFM yield was 98%. Finally, a synthesis strategy for the preparation of highly efficient Cu-based hydrogenation catalyst with optimized characteristics is suggested. [ABSTRACT FROM AUTHOR]