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<p>A robust heterogeneous palladium catalyst was constructed by immobilizing a 1,10-phenanthroline-Pd(II) complex onto mesoporous SBA-15 silica via post-synthetic surface functionalization. The catalyst, SBA-15@PHEN-Pd(II), was prepared through sequential silylation of SBA-15, covalent anchoring of 5-amino-1,10-phenanthroline, and subsequent coordination with PdCl<sub>2</sub>. Comprehensive characterization by TGA, XPS, atomic absorption spectroscopy (AAS), and Energy-dispersive X-ray spectroscopy (EDAX) confirmed successful surface modification and palladium immobilization. XPS analysis indicated that palladium is present in the + 2 oxidation state and coordinated to the phenanthroline nitrogens. SBA-15@PHEN-Pd(II) efficiently catalyzed CO-free carbonylation of aryl halides to carboxylic acids using a formic acid/DCC system. Systematic optimization identified DMF and NaOH at 120&#xa0;°C as optimal, enabling up to 76% yield across a broad substrate scope. Reactivity followed the order Ar-I &gt; Ar-Br &gt; Ar-Cl, and substrates bearing electron-withdrawing substituents exhibited enhanced reactivity. Negligible palladium leaching was observed, and hot filtration experiments confirmed the heterogeneous nature of the catalyst. SBA-15@PHEN-Pd(II) exhibits sustained catalytic activity over six consecutive cycles, highlighting its stability and efficiency as a CO-free carbonylation catalyst.</p>

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Efficient CO-free carbonylation of aryl halides catalyzed by SBA-15-supported Pd-1,10-phenanthroline

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年5月13日

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  • Maryam Fathinejad,
  • Yagoub Mansoori,
  • Somayeh Fekri,
  • Yuksel Akinay,
  • Tayfun Çetin

摘要

A robust heterogeneous palladium catalyst was constructed by immobilizing a 1,10-phenanthroline-Pd(II) complex onto mesoporous SBA-15 silica via post-synthetic surface functionalization. The catalyst, SBA-15@PHEN-Pd(II), was prepared through sequential silylation of SBA-15, covalent anchoring of 5-amino-1,10-phenanthroline, and subsequent coordination with PdCl2. Comprehensive characterization by TGA, XPS, atomic absorption spectroscopy (AAS), and Energy-dispersive X-ray spectroscopy (EDAX) confirmed successful surface modification and palladium immobilization. XPS analysis indicated that palladium is present in the + 2 oxidation state and coordinated to the phenanthroline nitrogens. SBA-15@PHEN-Pd(II) efficiently catalyzed CO-free carbonylation of aryl halides to carboxylic acids using a formic acid/DCC system. Systematic optimization identified DMF and NaOH at 120 °C as optimal, enabling up to 76% yield across a broad substrate scope. Reactivity followed the order Ar-I > Ar-Br > Ar-Cl, and substrates bearing electron-withdrawing substituents exhibited enhanced reactivity. Negligible palladium leaching was observed, and hot filtration experiments confirmed the heterogeneous nature of the catalyst. SBA-15@PHEN-Pd(II) exhibits sustained catalytic activity over six consecutive cycles, highlighting its stability and efficiency as a CO-free carbonylation catalyst.