Hemin immobilization in hydrophobic SBA15 as a Recyclable Catalyst for trans-selective Cyclopropanation in Aqueous Media

18 April 2025, Version 1
This content is a preprint and has not undergone peer review at the time of posting.

Abstract

Metal-porphyrin-based biocatalysts are gaining popularity in sustainable chemical synthesis. Heme-based enzymes like myoglobins, cytochrome P450s are known for their regio- and stereo-selective cyclopropanation reactions in aqueous media. However, their practical application is challenged by complex, multistep synthesis procedures and inherent structural instability. To address these limitations, we developed a stable, enzyme-mimicking heterogeneous catalyst using porous SBA-15 material. The inner core of SBA-15 was functionalized with an alkyl chain and protoporphyrin IX iron (III) (hemin), resulting in alkyl-SBA15-amideHemin. Characterization through TEM, UV-Vis, and FT-IR confirmed the successful immobilization of hemin within the hydrophobic pores of functionalized SBA-15. The catalytic performance of alkyl-SBA15-amideHemin was evaluated in the cyclopropanation reaction of styrene with ethyl diazoacetate (EDA), achieving a turnover number (TON) of 144—nearly double that of free hemin (TON 75). The catalyst exhibited high trans diastereoselectivity (~70%) for 2-(cyclopropyl benzene) esters in aqueous media, outperforming other known heterogeneous catalysts. Its catalytic activity and selectivity were maintained over four recycling cycles, highlighting its stability and reusability. Steady-state emission studies of the iron-carbene complex provided insights into the catalytic mechanism. These findings suggest that immobilized hemin within a hydrophobic environment serves as a robust and selective catalyst for chemical transformations in aqueous media.

Keywords

Enzyme mimic
Heterogeneous catalysis
Hemin
SBA-15
Carbene
Cyclopropanation
Iron carbene complex

Supplementary materials

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Title
Electronic Supplementary Information: Hemin immobilization in hydrophobic SBA15 as a Recyclable Catalyst for trans-selective Cyclopropanation in Aqueous Media
Description
This supplementary file provides detailed experimental procedures, characterization data, and catalytic analysis supporting the study titled "Hemin Immobilization in Hydrophobic SBA15 as a Recyclable Catalyst for trans-Selective Cyclopropanation in Aqueous Media." It includes the synthesis protocols of SBA-15 and its amine and alkyl-functionalized derivatives and procedures for covalently attaching Hemin to these supports. Comprehensive characterization via TEM, EDX, ICP-MS, FT-IR, BET, and UV-DRS confirms successful material modification and Hemin immobilization. The file also documents catalytic reactions using different alkyl-SBA15-Hemin systems with various diazoacetates and GC-MS and EI-MS data confirming product formation, stereoselectivity, and catalyst performance. Kinetic analyses, turnover calculations (TON, TOF), Calibration curves, and control experiments are also provided to validate product quantification and catalytic specificity. These data collectively support the efficiency, selectivity, and recyclability of the Prop-SBA15-amideHemin, one of the alkyl-SBA15-amideHemin catalysts for green cyclopropanation processes in water.
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