Facile One-pot Synthesis Research Articles

Facile one-pot synthesis of niobium-containing carbon nitride and the catalytic application for synthesis of dimethyl carbonate

Dimethyl carbonate (DMC) is a building block in wide chemical-related fields and the transesterification of ethylene carbonate (EC) and methanol/ethanol is a sustainable route for the synthesis of DMC. Herein, in order to explore efficient heterogeneous catalysts, niobium-containing carbon nitride materials were synthesized by a convenient one-pot calcination method. By reserving the main chemical functionalities of carbon nitride, the Nb-CN composites contained both acidic and basic properties, and Nb can be dispersed by carbon nitride. In the transesterification of EC with methanol, under the reaction temperature of 140 °C and reaction time of 4 h, the conversion of EC and the selectivity of DMC reached 53.8% and 100%, respectively, and the activity of the catalyst did not decrease significantly after several recycling runs. Furthermore, the Nb-CN could promote transesterification reactions of other cyclic carbonate and alcohols.

Facile one-pot synthesis of ternary Fe doped Cu-ZnO nanocatalyst: An efficient and recyclable solar light driven photocatalyst

Currently, nanoparticles are regarded as excellent materials for degrading and removing dyes due to their beneficial surface features and chemical reactivity. Herein, Cu doped ZnO (CZ) was co-doped with Fe (FCZ) at different concentrations (2, 3, 4 and 8 wt% with respect to CZ) via simple one-step co-precipitation approach. The structural, surface morphology, surface properties, optical and photocatalytic performance of prepared samples were studied. Due to the doping of Fe, the band gap of CZ reduced from 2.7 eV to 2.29 eV, which is beneficial for absorbing visible light. Among doped CZs, 4 wt% Fe-doped CZ (4FCZ) exhibited 97.1% methylene blue (MB) degradation at neutral pH under 60 min of sunlight exposure. Furthermore, the effect of initial concentration of dye, catalyst load, and pH on the degradation process was investigated. The remarkable photocatalytic activity of 4FCZ nanoparticles can be attributed to their advantageous surface properties, such as their high specific surface area, heterostructure morphology, and mesoporous nature. Scavenger study identified •O2−, e−, and h+ as main reactive species. Pseudo-first order kinetics revealed degradation order: 4FCZ>8FCZ>3FCZ>2FCZ>CZ. 4FCZ showed recyclability with 90.9% MB degradation after three cycles. Mineralization of MB was analysed by COD and LC-MS studies. Fe-doped CZ emerges as a promising, cost-effective wastewater treatment under sunlight without special equipment. This study provides new insights on synthesis of ternary nanocatalyst for dye degradation.

Copper-based nanodots as efficient biomimetic antibiotics for the treatment of oral bacterial infections

Oral infectious diseases caused by a variety of pathogenic bacteria seriously affect the quality of life. However, these diseases remain a clinical challenge because of the lack of simple, safe, and universal prophylactics. To address these limitations, we synthesize CuOx nanodots (CuOx NDs) with excellent Fenton-like reaction activity and utilize them in the treatment of oral bacterial infections. Different from other complicated approaches, CuOx NDs are rationally prepared using a facile one-pot aqueous synthesis. In the presence of H2O2, these well-developed CuOx NDs can efficiently catalyze the generation of hydroxyl radicals (·OH) around oral pathogens, leading to the death of various bacteria. Meanwhile, results of biosafety indicate the high biocompatibility and extremely low toxicity of these CuOx NDs. After understanding the admirable in vitro antibacterial effect of CuOx NDs in the presence of H2O2, we further explore their in vivo antibacterial performance on several classical animal models including oral mucosal wound model, intragingival bacteria-infected model, and the periodontal infection model. As expected, these CuOx NDs with wide-spectrum antibacterial activity can serve as high-performance antibacterial reagents for the treatment of various oral bacterial infections with the help of H2O2. In brief, current nanoplatform can act as efficient antibiotics against oral pathogens with broadening the biomedical applications of copper-based nanomaterials.

One-pot Synthesis of High-performance Green-emitting Carbon Dots for Cd2+ Sensing and Anti-counterfeiting Applications.

This study presents a facile one-pot solvothermal synthesis of high-performance green fluorescent carbon dots (G-CDs) using o-phenylenediamine and ethylenediamine as precursors. The G-CDs show excellent optical, temporal, and chemical stability. Notably, they exhibit the highest quantum yield of 24.2% in ethanol and a strong green emission peaking at 546nm under 440-490nm excitation. In addition, G-CDs have outstanding salt resistance and multi-solvent compatibility. Due to its bright photoluminescence, G-CDs can be used as a secure ink for anti-counterfeiting. More remarkably, Cd2+ ions can efficiently quench the fluorescence of G-CDs with a detection limit of 0.152 µmol/L, enabling accurate quantification of Cd2+ in water systems. The simple synthesis of high-performance G-CDs expands their applicability in sensing and bioimaging.

Simultaneous fingerprinting of multiplex collagen biomarkers in connective tissues by multicolor quantum dots-based peptide probes

The accurate detection of multiplex collagen biomarkers is vital for diagnosing and treating various critical diseases such as tumors and fibrosis. Despite the attractive optical properties of quantum dots (QDs), it remains technically challenging to create stable and specific QDs-based probes for multiplex biological imaging. We report for the first time the construction of multi-color QDs-based peptide probes for the simultaneous fingerprinting of multiplex collagen biomarkers in connective tissues. A bipeptide system composed of a glutathione (GSH) host peptide and a collagen-targeting guest peptide (CTP) has been developed, yielding CTP-QDs probes that exhibit exceptional luminescence stability when exposed to ultraviolet irradiation and mildly acidic conditions. The versatile bipeptide system allows for facile one-pot synthesis of high-quality multicolor CTP-QDs probes, exhibiting superior selectivity in targeting critical collagen biomarkers including denatured collagen, type I collagen, type II collagen, and type IV collagen. The multicolor CTP-QDs probes have demonstrated remarkable efficacy in simultaneously fingerprinting multiple collagen types in diverse connective tissues, irrespective of their status, whether affected by injury, diseases, or undergoing remodeling processes. The innovative multicolor CTP-QDs probes offer a robust toolkit for the multiplex fingerprinting of the collagen suprafamily, demonstrating significant potential in the diagnosis and treatment of collagen-related diseases.

Efficient green Cr(VI) adsorbent from sorghum waste: Eco-designed functionalized mesoporous silica FDU-12

This paper presents an eco-design approach to the synthesis of a highly efficient Cr(VI) adsorbent, utilizing a positively charged surface mesoporous FDU-12 material (designated as MI-Cl-FDU-12) for the first time. The MI-Cl-FDU-12 anion-exchange adsorbent was synthesized via a facile one-pot synthesis approach using sodium silicate extracted from sorghum waste as a green silica source, 1-methyl-3-(triethoxysilylpropyl) imidazolium chloride as a functionalization agent, triblock copolymer F127 as a templating or pore-directing agent, trimethyl benzene as a swelling agent, KCl as an additive, and water as a solvent. The synthesis method offers a sustainable and environmentally friendly approach to the production of a so-called “green” adsorbent with a bimodal micro-/mesoporous structure and a high surface area comparable with the previous reports regarding FDU-12 synthesis. MI-Cl-FDU-12 was applied as an anion exchanger for the adsorption of toxic Cr(VI) oxyanions from aqueous media and various kinetic and isotherm models were fitted to experimental data to propose the adsorption behavior of Cr(VI) on the adsorbent. Langmuir model revealed the best fit to the experimental data at four different temperatures, indicating a homogeneous surface site affinity. The theoretical maximum adsorption capacities of the adsorbent were found to be 363.5, 385.5, 409.0, and 416.9 mg g−1 at 298, 303, 308, and 313 K, respectively; at optimal conditions (pH=2, adsorbent dose=3.0 mg, and contact time of 30 min), surpassing that of most previously reported Cr(VI) adsorbents in the literature. A regeneration study revealed that this adsorbent possesses outstanding performance even after six consecutive recycling.

Facile One-Pot Synthesis and Anti-Microbial Activity of Novel 1,4-Dihydropyridine Derivatives in Aqueous Micellar Solution under Microwave Irradiation.

The current study describes a novel and eco-conscious method to synthesize 1,4-dihydropyridine derivatives utilizing an aqueous micellar solution containing aluminum dodecyl sulfate, Al(DS)3, using readily available starting material. The final products were synthesized with excellent yields within remarkably quick reaction durations, promoting remarkable atom economy and minimizing environmental impacts. The present protocol has several advantages over other methodologies in terms of high yield (up to 97%) with excellent purity. Further, the synthesized 1,4-DHPs exhibit favorable to excellent resistance against examined bacterial and fungal species. Intriguingly, polar groups on the phenyl ring (5b, 5c, 5i and 5j) make the 1,4-DHPs equally potent against the microbes as compared to the standard drugs.

Application of Green Synthesized Silver Nanoparticles for Dye Wastewater Treatment

A facile one-pot synthesis of silver nanoparticles (AgNPs) was achieved using the ethanolic extract of Cavendish banana florets as source of reducing agents for the conversion of Ag+ to Ag. The appearance of surface plasmon resonance peak between 410–435 nm in the UV Vis spectra confirmed the formation of AgNPs. The effects of different reaction conditions on the size and concentration of AgNPs were evaluated. The optimum conditions identified were pH 7 at 80 °C. Transmission electron microscopy (TEM) revealed spherical AgNPs with a mean particle size of 13.55 nm. On the other hand, energy-dispersive X-ray (EDX) analysis confirmed the presence of silver (Ag) as the bulk element (87.25%). Other elements such as carbon (C) and oxygen (O) are attributed to the capping agents of AgNPs which agrees with the results in the Fourier-transform infrared spectroscopy (FTIR) analysis. The optimized AgNPs were used for dye degradation using methyl orange (MO) as the model dye under acidified conditions. The maximum MO dye degradation of 96.07% and 77.32% at pH 1.5 and 2 were achieved after 10 min and 1320 min, respectively. This highlights the potential use of green-synthesized AgNPs for dye wastewater treatment.

Facile one-pot electrochemical synthesis and encapsulation of carbon quantum dots in GUVs

Water-soluble Carbon Quantum Dots (CQDs) featured with blue fluorescence were prepared by electrochemical synthesis at room temperature using carbon electrodes as a carbon source and encapsulated in liposomes of DMPC (1,2-dimyristoyl-sn‑glycero-3-phosphocholine) in a single quick step. The system liposome-CQDs was characterized by UV–vis absorption spectroscopy, fluorescence microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and epifluorescence microscopy. Electrochemical studies, such as cyclic voltammetry and impedance, have corroborated that electrosynthesis occurs at a voltage of -300 mV to form the hybrid system. The analysis includes the evaluation of variables with effect on the synthetic process of CQDs: voltage and reaction time. The results revealed that liposomes labeled with the CQDs are suitable for optical characterization by conventional and epifluorescence microscopies. In summary, this research involved the synthesis of water-soluble CQDs and their encapsulation in phospholipid vesicles in one pot, their characterization using various analytical techniques, the investigation of crucial synthesis variables, and particularly for visualization purposes in microscopy. Due to the rapidity and simplicity of the synthesis method, this work could have potential applications in analytical chemistry, biology, materials science, and related fields.

Facile Synthesis of 2-Substituted Quinazolines via Ruthenium(II)-Catalyzed Acceptorless Dehydrogenative Coupling

Abstract:: This study aims to develop a practical and facile one-pot synthesis of 2- substituted quinazolines. Using a commercially available and structurally simple ruthenium( II) complex as the catalyst to synthesize a series of quinazoline derivatives via acceptorless dehydrogenative coupling. The mechanism of this reaction was explored by control reaction and DFT calculation. This protocol offers access to a diverse array of quinazoline derivatives (52 examples) in moderate to excellent yields (29%-98%). In summary, we have developed an efficient one-pot ruthenium (II)-catalyzed ADC synthesis of quinazoline under an air atmosphere. The reaction only produces hydrogen and water as by-products, serving as a sustainable and atom-efficient synthetic approach.

In-Situ Derived Defective Ru Particles Anchored on Ru-Ni Layered Double Hydroxides for Enhanced Alkaline Hydrogen Evolution.

Developing active, stable, and cost-efficient electrocatalysts to replace platinum for the alkaline hydrogen evolution reaction (HER) is highly desirable yet represents a great challenge. Here, it is reported on a facile one-pot synthesis of RuxNi layered double hydroxides (RuxNi-LDHs) that exhibit remarkable HER activity and stability after an in-situ activation treatment, surpassing most state-of-the-art Ru-based catalysts as well as commercial Ru/C and Pt/C catalysts. The structural and chemical changes triggered by in-situ activation are systematically investigated, and the results clearly show that the pristine, less-active RuxNi-LDHs are transformed into a highly active catalyst characterized by raft-like, defect-rich Ru° particles decorated on the surface of RuxNi-LDHs. Density functional theory (DFT) calculations reveal that the defective Ru sites can effectively optimize the reaction pathway and lower the free energies of the elemental steps involved, leading to enhanced intrinsic activity. This work highlights the importance of the currently understudied strategy of defect engineering in boosting the HER activity of Ru-based catalysts and offers an effective approach involving in-situ electrochemical activation for the development of high-performance alkaline HER catalysts.

Facile one-pot synthesis of hydroxylated 1,3-dithiane-pyrazolone hybrids

Facile one-pot synthesis of hydroxylated 1,3-dithiane-pyrazolone hybrids

Crystal structure of a phenoxyl radical complex relevant to the metal site of the galactose oxidase enzyme: A facile one-pot synthesis, evidence for hydrogen atom transfer and DNA cleavage via self-activation.

Copper complexes [Cu(L1H)ClO4] (1) and [Cu(L2)NO3] (2), which are relevant to the metal site of the galactose oxidase enzyme, were synthesized and characterized by different spectroscopic methods. L1H2 and L2H2 [where L1H2 stands for 2,2'-((1E,1'E)(2,2'-(pyridine-2,6-diyl)bis(2-phenylhydrazin-2-yl-1-ylidene))bis(methanylylidene))diphenol and L2H2 stands for 6,6'-((1E,1'E)-(2,2'-(pyridine-2,6-diyl)bis(2-phenylhydrazin-2-yl-1-ylidene))bis(methanylylidene))bis(2,4-di-tert-butylphenol), H stands for dissociable proton] are pentadentate ligands. These ligands provide pyridyl N, two imine N, and two non-innocent phenoxyl and phenolato O donors, forming complex 1 as a non-radical complex, while complex 2 is a phenoxyl radical complex. The molecular structures of complexes 1 and 2 were authenticated by X-ray crystallography. Benzyl alcohol oxidation was investigated, and the conversion of 9,10-dihydroanthracene to anthracene was examined to scrutinize the H-atom abstraction reaction. Nuclease activity with complexes 1 and 2 was investigated by self-activated plasmid DNA (pBR322) cleavage. Non-innocent properties of the ligand-containing phenolato function were investigated by DFT calculations.

A facile one-pot synthesis of tetrahydrobenzo[b]pyrans and 2-amino-4H-chromenes under green conditions.

This research developed a new nanocatalyst by incorporating nanocopper iodide onto the surface of a layered double hydroxides modified. This new nanocatalyst enables the green synthesis of tetrahydrobenzo[b]pyrans and 2-amino-4H-chromene derivatives through a one-pot, three-component reaction, demonstrating remarkable activity and selectivity. Key advantages of this method include increased products yield (86-96%), rapid reaction kinetics (5-23 minutes), low reaction temperature (40 °C), synthesis of new products, straightforward purification methods, catalyst recyclability (up to 4 cycles), and solvent-free conditions.

Facile one-pot synthesis of a waste copper phthalocyanine-derived nanocomposite for efficiently removing dyes from wastewater

Water pollution from synthetic dyes is a growing environmental concern and there is an urgent need for the development of eco-friendly, cost-effective, rapid, simple, and effective materials for the extraction of these persistent dyes from effluents.

Facile one-pot synthesis of a manganese–cerium dual-doped hydroxyapatite nanocatalyst using Phyllanthus emblica extract for photocatalytic degradation of methylene blue dye and catalytic reduction of 4-nitrophenol

Novel Mn-Ce/HAp nanocatalyst was fabricated using green extract of Phyllanthus emblica and utilized it for the photodegradation of methylene blue dye and reduction of 4-NP to 4-AP.

Facile one-pot synthesis of the mesoporous chitosan-coated cobalt ferrite nanozyme as an antibacterial and MRI contrast agent.

Cobalt ferrite (CoFe) nanoparticles (NPs) with appropriate physicochemical and biological properties have attracted great attention for biomedical applications. In the present study, chitosan-coated mesoporous CoFe (CoFeCH) NPs were synthesized using a facile one-step hydrothermal method and fully characterized using FE-SEM, EDS, BET, FTIR spectroscopy, DLS, TGA, XRD, and VSM. The spherical, highly colloidal, and monodispersed CoFeCH NPs with an average hydrodynamic size of 177.9 nm, PDI of 0.238 and zeta potential value of -33 represented a high saturation magnetization value of 59.37 emu g-1. N2 adsorption-desorption analysis confirmed the mesoporous structure of CoFeCH NPs with a type IV isotherm, calculated specific surface area of 89.583 m2 g-1 and total pore volume of 0.3668 cm3 g-1. CoFeCH NPs exhibited high antibacterial effects on S. aureus and E. coli, comparable with standard antibiotics, while CH-coating led to higher biocompatibility of CoFe NPs on human cells in vitro. CoFeCH NPs also showed significant peroxidase activity with a Km value of 14.37 and specific activity of 0.632 mmol min-1. CoFeCH NPs were successfully used as a MRI contrast agent with an R2 value of 91.3 mM-1 s-1. The overall results indicated the high potential of synthesized CoFeCH NPs by the present method for biomedical applications, especially as an antibacterial and MRI contrast agent.

Facile one-pot synthesis of novel imidates as multifunctional organic fluorescent materials

A novel one-pot synthesis of multifunctional organic fluorescent imidates from quinolinium salt derivatives, nitrosoarenes and alcohols was presented. This method had a wide substrate scope and excellent isolated yields.

A one-pot synthesis of 2,3-dihydrobenzofurans, benzofuran-2(3H)-ones, and indoles via a [4 + 1] annulation reaction of ortho-substituted para-quinone methides and bromonitromethane.

Under mild and metal-free reaction conditions, a facile one-pot synthesis of oxygen- and nitrogen-containing benzoheterocycles has been achieved through [4 + 1] annulation of para-quinone methides, followed by an oxidation/elimination sequence, efficiently synthesizing functionalized 2,3-dihydrobenzofuran, benzofuran-2(3H)-one, and indole derivatives in moderate to good yields (up to 72%). A novel functional group tolerant oxidative Nef reaction utilizes DDQ without a base.

Facile one-pot synthesis of flower-like ellagic acid microparticles incorporating anti-microbial peptides for enhanced wound healing.

Anti-microbial peptides (AMPs) have gained significant attention as potential antimicrobial agents due to their cytocompatibility and reduced drug resistance. However, AMPs often suffer from low stability due to their vulnerable molecular structure. This study presents a one-pot synthesis method for ellagic acid (EA)-based, flower-like AMPs@EAMP particles, combining the antibacterial properties of EA with AMPs. The resulting particles exhibit an enlarged surface area for the adsorption or embedding of AMPs, enhancing their antibacterial efficacy. Furthermore, in vitro evaluations demonstrate excellent biocompatibility and broad-spectrum activity against bacterial strains including both Gram-positive S. epidermidis and Gram-negative E. coli. In vivo studies indicate AMPs@EAMPs' potential to reconstruct the immune barrier, inhibit pathogens, and reduce inflammation, promoting orderly tissue repair. This innovative synthesis strategy provides a straightforward and effective approach for large-scale production of flower-like AMPs@EAMP particles with remarkable antibacterial properties, addressing the challenges associated with MDR infections.