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article
H5PW10V2O40@VOx/SBA-15-NH2 catalyst for the solventless synthesis of 3-substituted indoles
Abstract
Functionalization of mesoporous SBA-15 frameworks by transition metal oxides offers a flexible route to fabricate new heterogeneous catalysts. Here, an inorganic-organic hybrid nanoporous catalyst H<sub>5</sub>PW<sub>10</sub>V<sub>2</sub>O<sub>40</sub>@VO<sub>x</sub>/SBA-15-NH<sub>2</sub>, was prepared and utilized as an efficient, eco-friendly, and recyclable catalyst for the one-pot, multi-component synthesis of 3-substituted indoles by indole substitution with aldehydes and malononitrile under solvent-free conditions. Catalysts were prepared by the non-covalent attachment of H<sub>5</sub>PW<sub>10</sub>V<sub>2</sub>O<sub>40</sub> to a 3 wt%VO<sub>x</sub>/SBA-15 nanoporous support through a 3-(triethoxysilyl)propylamine linker. VO<sub>x</sub>/SBA-15 was prepared by a one-pot hydrothermal synthesis from TEOS and vanadium(V) oxytri-tert-butoxide [VO(O<sup>-t</sup>Bu)3]. The resulting H<sub>5</sub>PW<sub>10</sub>V<sub>2</sub>O<sub>40</sub>@VO<sub>x</sub>/SBA-15-NH<sub>2</sub> material was characterized by bulk and surface analysis including N2 porosimetry, FE-SEM, XRD, XPS, FT-IR, TGA-DTA, UV–Vis and ICP-OES, evidencing retention of the heteropolyacid Keggin structure. H<sub>5</sub>PW<sub>10</sub>V<sub>2</sub>O<sub>40</sub>@VO<sub>x</sub>/SBA-15-NH<sub>2</sub> exhibits high activity and excellent yields (70–95%) of 3-substituted indoles under mild conditions, with negligible deactivation.