Research on Chemical Intermediates最新文献

The synthesis of bioactive chromene derivatives is of great significance due to their diverse pharmacological properties. In this study, a novel magnetically recoverable nanocatalyst, Fe₃O₄-β-cyclodextrin-graphene oxide (Fe₃O₄-β-CD-GO), was developed and thoroughly characterized using techniques such as Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Fourier-Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA), and Vibrating Sample Magnetometer (VSM), confirming its successful fabrication, stability, and magnetic properties. This heterogeneous catalyst was employed for the efficient and green synthesis of 2-amino-3-cyano-4H-chromenes in aqueous media at 80 °C, showing excellent yields up to 95% within short reaction times (10–60 min). Optimization studies highlighted the superior performance of water as a solvent, with catalyst loading (0.7 mol%) and temperature significantly influencing reaction efficiency. The catalyst demonstrated remarkable recyclability, maintaining high activity over at least eight cycles, facilitated by easy magnetic separation. A plausible reaction mechanism was proposed, involving activation of electrophiles and nucleophiles via hydrogen bonding and acid–base interactions. The method proved versatile, accommodating various aldehyde substrates with different electronic properties, and scalable for larger-scale synthesis. These findings underscore the catalyst’s potential for sustainable, cost-effective, and efficient organic transformations, advancing green chemistry protocols in pharmaceutical and material synthesis.

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Benzyl alcohol (BOL), an aromatic compound bearing oxygen-containing functional groups, is capable of forming BOL-based hyper-cross-linked resin (BOL-HCPs) with chloromethylated polystyrene resins (CMPs) via a sequence of chemical reactions. A combination of characterization techniques, including BET, FT-IR, SEM-Mapping, XPS, XRD, contact angle measurement, and TGA, was confirmed the successful preparation of the adsorbent. Notably, the incorporation of BOL significantly increases both the specific surface area (S_BET) and hydrophilicity of the adsorbent. BOL-HCPs, prepared by Friedel–Crafts alkylation and nucleophilic substitution reaction, exhibited excellent phenol removal capacity from aqueous solutions. The Langmuir isotherm model better describes the resin’s equilibrium adsorption, showing a max capacity of 275.2 mg/g at 298 K. Kinetic analysis reveals that the adsorption of pollutants reaches equilibrium rapidly within 90 min, which is consistent with the pseudo-first-order model. Owing to its favorable S_BET, abundant micropores/mesopores, as well as hydrogen bonding interactions, the adsorbent enables highly efficient phenol adsorption. This work offers a new strategy for phenol removal from aqueous solutions.

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This study outlines an easy, efficient and environmentally sustainable method for the green synthesis of manganese dioxide (MnO₂) nanoparticles using an extract from Psidium guajava leaves. The catalytic activity of MnO₂@Ag–S–CH₂–COOH nanocatalyst was explored for the one-pot synthesis of hydrazinyl thiazole derivatives, utilizing a three-component reaction involving different aryl aldehydes, phenacyl bromides, and thiosemicarbazide. A number of techniques were used to characterize the MnO₂@Ag–S–CH₂–COOH nanocatalyst, field emission scanning electron microscopy (FE-SEM), Brunner–Emmett–Teller (BET), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), and energy-dispersive X-ray (EDX). The structures of each newly synthesized derivative of hydrazinyl thiazole have been confirmed via the use of nuclear magnetic resonance (¹H and ¹³C NMR), fourier-transform infrared (FTIR) and high resolution mass spectrometry (HRMS). The MnO₂@Ag–S–CH₂–COOH nanocatalyst was readily extracted from the reactions with the use of an external magnet and could be reused five times without experiencing a substantial loss in efficacy. The synthesized compounds demonstrated promising results when assessed in vitro for their antimicrobial and anticancer activities. The anticancer efficacy of the synthesized hydrazinyl thiazole compounds were assessed in vitro against the MCF-7 human breast cancer cell line using the MTT assay. Among them, compounds 4a and 4e exhibited notable anticancer effects, with IC₅₀ values of 82.30 ± 0.58 and 84.25 ± 0.28 μg/mL respectively.

A series of Pt-based catalysts supported on morphology-controlled ZSM-5 zeolites were synthesized and applied for toluene catalytic oxidation. The results demonstrated that the catalyst Pt supported on sheet-like ZSM-5 (Pt/S-ZSM) exhibited significantly higher activity than those supported on chain-like ZSM-5 (Pt/C-ZSM) and unmodified ZSM-5 (Pt/N-ZSM). The sheet-like morphology ZSM-5 zeolites exhibited a toluene saturation capacity of 65.17 mg·g⁻¹, with breakthrough time and saturation adsorption increased by 2.4-fold and 1.4-fold, respectively, compared to unmodified N-ZSM-5. Notably, compared to 0.5wt% Pt/C-ZSM, the 0.5wt% Pt/S-ZSM catalyst exhibited a significantly lower apparent activation energy (11.63 kJ·mol⁻¹), confirming the superior suitability of S-ZSM as a Pt support. This was further evidenced by its exceptional catalytic activity, achieving 90% toluene conversion (T₉₀) at just 181℃. The Pt/S-ZSM showed well catalytic activity and structural stability during the toluene catalytic combustion, which reflected a promising catalyst for practical application.

A new mixed ligands Cobalt complex of Schiff base and 2,2′-bipyridine was anchored onto the mesoporous MCM-41 to synthesize a highly efficient and reusable heterogeneous catalyst. The prepared heterogeneous catalyst was characterized by FT-IR, UV-DRS, PXRD, SEM-EDX, ICP-OES, HR-TEM, TGA, N₂ adsorption and desorption and ¹³C-CP-MAS-NMR. The Salen-Co-MCM-41-bipy complex has been found as a more promising catalyst for Knoevenagel condensation of aryl/alkyl malononitriles using different kind of aldehydes with malononitrile in EtOH/H₂O solvent mixture under room temperature with the yield upto 99%. The catalyst was performed well against a wide range of substrates, viz, the aldehydes of aryl, fused aryl, hetero and aliphatic compounds with a variety of substituents at various positions. Moreover, the effectiveness of our catalyst against large-scale reaction up to 2.5 g of substrate was also explained. The catalyst is recovered by simple filtration and reused up to five times without any loss in activity. Hot filtration test was explored the heterogeneous nature of the recovered catalyst. Previous reports were compared and discussed to spotlight the efficiency of our catalyst.

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Sulfated trishydroxyaminomethane has been found to be an efficient solid acid catalyst for the solvent-free synthesis of bisindolylmethanes. This innovative catalytic approach’s attractive features include its sustainability, ease of workup, economic viability, and biodegradability. The sulfonated trishydroxyaminomethane catalyst was assessed using infrared spectroscopy, scanning electron microscopy, wide-angle X-ray scattering analysis, and nuclear magnetic spectroscopy analysis. The results clearly show that sulfonation has been functionalized. The catalyst could be reused six times without exhibiting a discernible drop in activity. Furthermore, chromatographic separations may not be required to achieve the desired products with good yields.

Zinc oxide (ZnO) nanoparticles have been identified as a highly efficient and recyclable catalyst for the microwave-assisted synthesis of 1,8-dioxooctahydroxanthenes in an ethanol solvent medium. In this study, ZnO nanoparticles were synthesized via a green approach using Mirabilis Jalapa flower extract as a natural reducing agent, offering an eco-friendly and sustainable alternative to conventional chemical methods.The nanoparticles were thoroughly characterized using ultraviolet–visible (UV–vis) spectroscopy, Field-Emission Scanning Electron Microscopy (FE-SEM), Transmission Electron Microscope (TEM), Energy Dispersive X-ray analysis (EDX), Elemental Mapping, X-ray diffraction (XRD), Thermogravimetric analysis (TGA), X-ray Photoelectron Spectroscopy (XPS) analyses and Fourier Transform Infrared Spectroscopy (FTIR), Brunauer–Emmett–Teller (BET) analysis. X-ray diffraction (XRD) results confirmed the formation of a crystalline hexagonal wurtzite structure. The catalyst demonstrated excellent recyclability, being easily recovered through simple filtration and reused for up to five consecutive cycles without significant loss of efficiency. This nanostructure-based heterogeneous catalytic protocol is not only sustainable and environmentally friendly but also economically advantageous due to the high recyclability of the catalyst.

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The synthesis of 2,4,5-substituted imidazoles has garnered significant attention due to the diverse biological activities exhibited by these compounds. In this study, we report a novel approach utilizing copper ferrite-coated silica–titania nanocomposites, CuFe₂O₄@SiO₂.TiO₂, as an efficient catalyst for the one-pot synthesis of 2,4,5-substituted imidazoles. The reaction protocol involves the condensation of aryl aldehydes, benzil, and an ammonia source (ammonium acetate) under mild conditions. The synthesized nanocomposite catalyst demonstrates impressively high catalytic activity and selectivity, achieving good yields of the desired imidazole derivatives. Comprehensive characterization of the nanocomposites using techniques such as FT-IR, XRD, SEM, and TEM confirmed the successful synthesis and morphology of the catalyst. The catalyst’s effectiveness highlighted its recyclability and stability over six reaction cycles, making it a promising candidate for green synthetic methodologies. The optimized reaction conditions achieved excellent yields within a short reaction time and showcased the potential of this nanocomposite in facilitating green chemistry practices. This work highlights that the versatility of CuFe₂O₄@SiO₂.TiO₂ nanocomposites in organic synthesis opens new avenues for developing efficient catalytic systems to prepare biologically significant heterocycles, instilling hope for a more sustainable future in the field of chemistry.

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In developing effective catalytic systems, understanding the interaction between reactant(s) and organocatalysts plays a crucial role in establishing the structure–activity relationship (SAR) in catalysis. This work investigated the interaction between imidazole, an organocatalyst, with the reactants in the Knoevenagel condensation of 2-chlorobenzaldehyde with malononitrile and ethyl cyanoacetate. Due to the solvent's impact on plausible interactions between reactants, organocatalysts, and intermediates, the study was conducted using FTIR and 1D NMR spectroscopic techniques. There was a correlation between the reduction of the acid methylene group intensity in ¹³C NMR spectra and the activity of acid methylene compounds. A reduction in α-carbon intensity of 75% and 23% for the malononitrile and ethyl cyanoacetate, respectively, was observed in the presence of one equivalent of imidazole. Moreover, the study introduced a greener and more sustainable solid-state procedure for the gram-scale preparation of 2-chlorobenzylidene malononitrile and 2-chlorobenzylidene cyanoacetic acid ethyl ester using a catalytic loading of imidazole, demonstrating the economic and practical aspects of the slurry mechanochemical process. The crystalline pure products could be isolated directly from an ethanol solution, and the residue containing imidazole was used in the next reactions without purification or activation after removing ethanol with a rotary evaporator.

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