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Organo-modified Fe-montmorillonite as a solid acid catalyst for reduction of nitroarenes and Biginelli reactions
Abstract In order to develop a new class of solid acid catalysts, interlayer ferric ions of Fe(III)-montmorillonite (Mt) was reduced to Fe2+ and coordinated with o-phenanthroline (L) during the solid-state reaction at >150 °C. Such a reduction is ascribed to the partial aggregation of Fe3+–O-Fe3+ followed by self-reduction to Fe2+ with the elimination of oxide ion. In-situ complexation to form ferroin, [FeL3]2+ at the interlayer is evident from TG/DTA, DR UV–Vis spectra, XRD, FT-IR, photoluminescence spectra and SQUID magnetometer. Basal spacing (d 001) of Fe(III)-Mt-L was 18 Å for the products heated from 200 to 350 °C. The decomposition of this interlayer complex occurred around 450 °C. Fe(III)-Mt-L@200 °C showed characteristic absorption for [FeL3]2+ around 510 nm. Lewis and Brønsted acid sites are confirmed from the FTIR spectra of pyridine adsorbed samples. The catalytic behavior of Fe(III)-Mt-L@300 °C was observed during the reduction of 4-nitrophenol to 4-aminophenol and also in the Biginelli reactions.
Graphical abstract Display Omitted
Highlights Fe3+ → Fe2+ occurred in the interlayer of Fe(III)-Mt with o-phen (L) @ T > 150 °C. Increase in d001 = 18 Å is due to formation of in-situ complex, [FeL3]2+. Fe(III)-Mt-L showed Bronsted and Lewis acid sites and stable up to 350 °C. Fe(III)-Mt-L@ 200 °C, 300 °C and 400 °C showed paramagnetic behavior. Reduction of 4-NP to 4-AP occurred with NaBH4 in presence of Fe(III)-Mt-L@300 °C.
Organo-modified Fe-montmorillonite as a solid acid catalyst for reduction of nitroarenes and Biginelli reactions
Abstract In order to develop a new class of solid acid catalysts, interlayer ferric ions of Fe(III)-montmorillonite (Mt) was reduced to Fe2+ and coordinated with o-phenanthroline (L) during the solid-state reaction at >150 °C. Such a reduction is ascribed to the partial aggregation of Fe3+–O-Fe3+ followed by self-reduction to Fe2+ with the elimination of oxide ion. In-situ complexation to form ferroin, [FeL3]2+ at the interlayer is evident from TG/DTA, DR UV–Vis spectra, XRD, FT-IR, photoluminescence spectra and SQUID magnetometer. Basal spacing (d 001) of Fe(III)-Mt-L was 18 Å for the products heated from 200 to 350 °C. The decomposition of this interlayer complex occurred around 450 °C. Fe(III)-Mt-L@200 °C showed characteristic absorption for [FeL3]2+ around 510 nm. Lewis and Brønsted acid sites are confirmed from the FTIR spectra of pyridine adsorbed samples. The catalytic behavior of Fe(III)-Mt-L@300 °C was observed during the reduction of 4-nitrophenol to 4-aminophenol and also in the Biginelli reactions.
Graphical abstract Display Omitted
Highlights Fe3+ → Fe2+ occurred in the interlayer of Fe(III)-Mt with o-phen (L) @ T > 150 °C. Increase in d001 = 18 Å is due to formation of in-situ complex, [FeL3]2+. Fe(III)-Mt-L showed Bronsted and Lewis acid sites and stable up to 350 °C. Fe(III)-Mt-L@ 200 °C, 300 °C and 400 °C showed paramagnetic behavior. Reduction of 4-NP to 4-AP occurred with NaBH4 in presence of Fe(III)-Mt-L@300 °C.
Organo-modified Fe-montmorillonite as a solid acid catalyst for reduction of nitroarenes and Biginelli reactions
Kabadagi, Anand (author) / Chikkamath, Santosh (author) / Kobayashi, Satoru (author) / Manjanna, Jayappa (author)
Applied Clay Science ; 189
2020-02-13
Article (Journal)
Electronic Resource
English
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