What question did this study set out to answer?

To develop a CO-free method for the carbonylation of aryl halides using a palladium catalyst supported on SBA-15.

May 16, 2026Scientific Reports0 citationsOpen Access

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

MFMaryam FathinejadUniversity of Mohaghegh Ardabili YMYagoub MansooriUniversity of Mohaghegh Ardabili SFSomayeh FekriUniversity of Mohaghegh Ardabili

Key Points

To develop a CO-free method for the carbonylation of aryl halides using a palladium catalyst supported on SBA-15.
Palladium immobilization on SBA-15 was characterized using TGA, XPS, AAS, and EDAX.
The reaction was optimized using DMF and NaOH at 120 °C to achieve high yields of carboxylic acids.
Catalyst performance was assessed across multiple cycles to evaluate stability and reusability.
Achieved up to 76% yield of carboxylic acids from aryl halides under optimal conditions.
Reactivity order was Ar-I > Ar-Br > Ar-Cl, with electron-withdrawing substituents enhancing reactivity.
Negligible palladium leaching and sustained catalytic activity over six cycles were confirmed.

Abstract

. 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.

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