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<p>In this work, an eco-friendly and efficient heterogeneous catalyst based on LaCoO<sub>3</sub> perovskite supported on montmorillonite clay was synthesized and applied to the solvent-free Biginelli reaction for the preparation of 3,4-dihydropyrimidin-2(1H)-one (DHPM). Structural, textural, and acidic properties were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), N<sub>2</sub> physisorption (BET/BJH), and pyridine-adsorbed FTIR spectroscopy. These analyses confirmed the successful formation of the composite, the preservation of the perovskite phase, the homogeneous dispersion of LaCoO<sub>3</sub> nanoparticles, its mesoporous nature, and the presence of both Brønsted and Lewis acid sites. The synthesized DHPM product was characterized by NMR, IR spectroscopy, and high-resolution mass spectrometry (HRMS), in addition to melting point determination, confirming its structure and high purity. The catalytic performance was optimized using a Box–Behnken design (BBD) by varying catalyst amount, reaction time, and temperature. Under the optimal conditions (8&#xa0;wt% catalyst relative to benzaldehyde, 4&#xa0;h, and 90.3&#xa0;°C), a maximum yield of 96.7% was obtained. The catalyst exhibited excellent recyclability over several consecutive runs with negligible loss of activity, while hot filtration experiments confirmed its heterogeneous nature. These results demonstrate that the LaCoO<sub>3</sub>/montmorillonite composite is an efficient and sustainable catalyst for green multicomponent synthesis under solvent-free conditions.</p>

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Solvent-free synthesis of a Biginelli-derived heterocycle over a LaCoO3/montmorillonite composite catalyst: optimization via Box–Behnken design

  • 期刊论文

  • 发表日期：

    2026年7月13日

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  • Souaad Khodja,
  • Farida Bouremmad,
  • Lamia Bouchenka,
  • Fatine Djabelkhir,
  • Fatima Zohra Akika,
  • Ivalina Avramova,
  • Fulvia Felluga,
  • Federico Berti

摘要

In this work, an eco-friendly and efficient heterogeneous catalyst based on LaCoO3 perovskite supported on montmorillonite clay was synthesized and applied to the solvent-free Biginelli reaction for the preparation of 3,4-dihydropyrimidin-2(1H)-one (DHPM). Structural, textural, and acidic properties were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), N2 physisorption (BET/BJH), and pyridine-adsorbed FTIR spectroscopy. These analyses confirmed the successful formation of the composite, the preservation of the perovskite phase, the homogeneous dispersion of LaCoO3 nanoparticles, its mesoporous nature, and the presence of both Brønsted and Lewis acid sites. The synthesized DHPM product was characterized by NMR, IR spectroscopy, and high-resolution mass spectrometry (HRMS), in addition to melting point determination, confirming its structure and high purity. The catalytic performance was optimized using a Box–Behnken design (BBD) by varying catalyst amount, reaction time, and temperature. Under the optimal conditions (8 wt% catalyst relative to benzaldehyde, 4 h, and 90.3 °C), a maximum yield of 96.7% was obtained. The catalyst exhibited excellent recyclability over several consecutive runs with negligible loss of activity, while hot filtration experiments confirmed its heterogeneous nature. These results demonstrate that the LaCoO3/montmorillonite composite is an efficient and sustainable catalyst for green multicomponent synthesis under solvent-free conditions.