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<p>Amide formation through the Ritter reaction remains a valuable transformation in pharmaceutical and materials chemistry, yet conventional protocols rely heavily on corrosive homogeneous acids and non-green conditions. In this study, a magnetite nanoparticles/graphitic carbon nitride/ nitrilotri(methylphosphonic acid (Fe<sub>3</sub>O<sub>4</sub>/g-C<sub>3</sub>N<sub>4</sub>/NTMPA) magnetic nanocomposite (MNC) was synthesized via a co-precipitation method and employed as an efficient and recyclable solid acid catalyst for solvent-free Ritter reactions at 80&#xa0;°C. Structural and morphological analyses using FT-IR, XRD, FE-SEM, TEM, DLS, and EDX confirmed successful incorporation of NTMPA and uniform distribution of Fe, C, N, O, and P throughout the composite. BET analysis showed a surface area of 11.421&#xa0;m<sup>2</sup>/g, pore volume of 0.0588&#xa0;cm³/g, and mean pore diameter of 20.593&#xa0;nm, indicating a mesoporous structure conducive to catalytic accessibility. TGA revealed a major decomposition step of 23.88% between 500 and 600&#xa0;°C corresponding to g-C<sub>3</sub>N<sub>4</sub> degradation, confirming appropriate thermal stability. The catalyst demonstrated broad substrate applicability, converting tertiary alcohols and benzylic alcohols to the corresponding amides in high to excellent yields in 1.25–6&#xa0;h. Aromatic nitriles consistently delivered yields above 90% within 5–6&#xa0;h, with electron-withdrawing substituents further enhancing reactivity and aliphatic nitriles provide the related amides in 87–98% yields within 1.5–5.5&#xa0;h. The catalyst retained over 90% activity after six cycles, with post-reaction analyses confirming structural integrity. These results highlight Fe<sub>3</sub>O<sub>4</sub>/g-C<sub>3</sub>N<sub>4</sub>/NTMPA as a robust, magnetically recoverable, and environmentally compatible catalyst for green amide synthesis.</p>

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Efficient solvent-free amide synthesis via Ritter reaction catalyzed by a reusable Fe3O4/g-C3N4/ NTMPA nanocomposite

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  • 发表日期：

    2026年1月28日

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  • Haniehsadat Karimitabar,
  • Ali Reza Sardarian

摘要

Amide formation through the Ritter reaction remains a valuable transformation in pharmaceutical and materials chemistry, yet conventional protocols rely heavily on corrosive homogeneous acids and non-green conditions. In this study, a magnetite nanoparticles/graphitic carbon nitride/ nitrilotri(methylphosphonic acid (Fe3O4/g-C3N4/NTMPA) magnetic nanocomposite (MNC) was synthesized via a co-precipitation method and employed as an efficient and recyclable solid acid catalyst for solvent-free Ritter reactions at 80 °C. Structural and morphological analyses using FT-IR, XRD, FE-SEM, TEM, DLS, and EDX confirmed successful incorporation of NTMPA and uniform distribution of Fe, C, N, O, and P throughout the composite. BET analysis showed a surface area of 11.421 m2/g, pore volume of 0.0588 cm³/g, and mean pore diameter of 20.593 nm, indicating a mesoporous structure conducive to catalytic accessibility. TGA revealed a major decomposition step of 23.88% between 500 and 600 °C corresponding to g-C3N4 degradation, confirming appropriate thermal stability. The catalyst demonstrated broad substrate applicability, converting tertiary alcohols and benzylic alcohols to the corresponding amides in high to excellent yields in 1.25–6 h. Aromatic nitriles consistently delivered yields above 90% within 5–6 h, with electron-withdrawing substituents further enhancing reactivity and aliphatic nitriles provide the related amides in 87–98% yields within 1.5–5.5 h. The catalyst retained over 90% activity after six cycles, with post-reaction analyses confirming structural integrity. These results highlight Fe3O4/g-C3N4/NTMPA as a robust, magnetically recoverable, and environmentally compatible catalyst for green amide synthesis.