Microwave-Assisted, Solvent-Free Synthesis of Benzothiazoles Using a Bimetallic Fe–Al/Silica Heterogeneous Catalyst

Objective: Green chemistry emphasizes the development of efficient, sustainable, and environmentally friendly catalytic systems. The present study aimed to design and evaluate a bime-tallic Fe–Al/silica heterogeneous catalyst for the microwave-assisted, solvent-free synthesis of ben-zothiazoles, addressing the limitations of conventional homogeneous and monometallic catalytic systems. Methods: The Fe–Al/silica catalyst was prepared by co-impregnation of Fe and Al precursors onto silica, followed by calcination. Its structural and morphological characteristics were analyzed using XRD, FT-IR, SEM, and EDS. Catalytic performance was assessed by the condensation of 2-ami-nothiophenol with aldehydes under microwave irradiation. Reaction parameters, including temper-ature, catalyst loading, and microwave power, were optimized. Comparative studies were per-formed against bare silica, monometallic, bimetallic, and homogeneous catalysts. Catalyst recycla-bility was evaluated through repeated cycles and hot-filtration tests. Results: Under optimized conditions (560 W, 120℃, 1.18 mol% catalyst), the Fe–Al/silica catalyst achieved up to 95% yield of benzothiazoles within 5 minutes, significantly outperforming control catalysts. The synergistic interaction of Fe (redox activity) and Al (Lewis acidity), uniformly dis-persed on silica, was identified as the key factor for enhanced activity and selectivity. The catalyst maintained >90% activity over seven reuse cycles with negligible leaching (<0.5% by ICP analy-sis). Discussion: The study highlights the superiority of Fe–Al/silica over conventional homogeneous salts (FeCl₃, AlCl₃) and other supported systems, owing to its high surface area, dual functional sites, and efficient microwave absorption. The cooperative effect between Fe and Al enhances cat-alytic efficiency while ensuring recyclability, aligning with green chemistry principles. Conclusion: This work demonstrates, for the first time, the efficiency of a recyclable Fe–Al/silica heterogeneous catalyst for solvent-free, microwave-assisted synthesis of benzothiazoles. The method offers rapid reaction times, high yields, energy efficiency, and environmental safety, providing a promising green alternative for heterocyclic synthesis.

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Publication Details

Journal
Current Organocatalysis
Published
2026-01-07
DOI
https://doi.org/10.2174/0122133372421830251119053531
Primary Topic
Multicomponent Synthesis of Heterocycles
Type
article
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article

Microwave-Assisted, Solvent-Free Synthesis of Benzothiazoles Using a Bimetallic Fe–Al/Silica Heterogeneous Catalyst

Nidhi Srivastava, Karuna Shanker Shukla, Rajni Devi, Bashir Ahmad Dar
Current Organocatalysis
Multicomponent Synthesis of Heterocycles
article

Microwave-Assisted, Solvent-Free Synthesis of Benzothiazoles Using a Bimetallic Fe–Al/Silica Heterogeneous Catalyst

Nidhi Srivastava, Karuna Shanker Shukla, Rajni Devi, Bashir Ahmad Dar
article en

Abstract

Objective: Green chemistry emphasizes the development of efficient, sustainable, and environmentally friendly catalytic systems. The present study aimed to design and evaluate a bime-tallic Fe–Al/silica heterogeneous catalyst for the microwave-assisted, solvent-free synthesis of ben-zothiazoles, addressing the limitations of conventional homogeneous and monometallic catalytic systems. Methods: The Fe–Al/silica catalyst was prepared by co-impregnation of Fe and Al precursors onto silica, followed by calcination. Its structural and morphological characteristics were analyzed using XRD, FT-IR, SEM, and EDS. Catalytic performance was assessed by the condensation of 2-ami-nothiophenol with aldehydes under microwave irradiation. Reaction parameters, including temper-ature, catalyst loading, and microwave power, were optimized. Comparative studies were per-formed against bare silica, monometallic, bimetallic, and homogeneous catalysts. Catalyst recycla-bility was evaluated through repeated cycles and hot-filtration tests. Results: Under optimized conditions (560 W, 120℃, 1.18 mol% catalyst), the Fe–Al/silica catalyst achieved up to 95% yield of benzothiazoles within 5 minutes, significantly outperforming control catalysts. The synergistic interaction of Fe (redox activity) and Al (Lewis acidity), uniformly dis-persed on silica, was identified as the key factor for enhanced activity and selectivity. The catalyst maintained >90% activity over seven reuse cycles with negligible leaching (<0.5% by ICP analy-sis). Discussion: The study highlights the superiority of Fe–Al/silica over conventional homogeneous salts (FeCl₃, AlCl₃) and other supported systems, owing to its high surface area, dual functional sites, and efficient microwave absorption. The cooperative effect between Fe and Al enhances cat-alytic efficiency while ensuring recyclability, aligning with green chemistry principles. Conclusion: This work demonstrates, for the first time, the efficiency of a recyclable Fe–Al/silica heterogeneous catalyst for solvent-free, microwave-assisted synthesis of benzothiazoles. The method offers rapid reaction times, high yields, energy efficiency, and environmental safety, providing a promising green alternative for heterocyclic synthesis.

Current OrganocatalysisVol. 13
Government of West Bengal (IN), Maharishi University of Management and Technology (IN), Hindu College of Pharmacy (IN)
Responsible consumption and production
Openalex Percentile: Top 93%
Multicomponent Synthesis of Heterocycles
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