One-pot Research Articles

Synthesis of high-entropy perovskite metal fluoride anode materials for lithium-ion batteries via a one-pot solution method

Synthesis of high-entropy perovskite metal fluoride anode materials for lithium-ion batteries via a one-pot solution method

Effective magnetic nanoadsorbent based on natural carboxymethyl cellulose/polyaniline nanotube/graphene oxide for aflatoxin B1 and B2 adsorption in rice utilizing a novel synthesis method

A magnetic nanoadsorbent was prepared via a novel one-pot magnetization method by employing natural carboxymethyl cellulose (CMC), polyaniline (PANI) nanotube, and graphene oxide (GO) for the effective adsorption of aflatoxins B1 (AFB1) and B2 (AFB2) from rice samples. This synthesized adsorbent combines the multifunction of CMC, PANI, and GO and shows improved extraction performance. FT-IR, XRD, FE-SEM, VSM, and TGA analyses were used to investigate the successful synthesis of the nanocomposite. The adsorption mechanism was ascribed to π-π interactions, hydrogen bonding, and hydrophobic interactions. Under optimized conditions, the method achieved extraction recoveries ranging from 78 % to 89 %. Low limits of detection (LODs) and quantification (LOQs) were obtained in the ranges of 0.07 and 0.01 ng g−1, and 0.20 and 0.04 ng g−1 for AFB1 and B2, respectively. This method showed an acceptable precision with intra- and inter-day relative standard deviations (RSDs) of less than 15 %. Comparative studies with other adsorbents used in extraction methods such as solid phase extraction (SPE), magnetic dispersive solid phase extraction (MDSPE), and matrix solid-phase dispersion (MSPD) demonstrated that the proposed method outperforms the existing procedures; it is promising in efficient AFs monitoring in rice.

A Novel pH-Responsive Nano-Sized Lanthanum-Doped Polyvinyl Alcohol-Carbon Quantum Dot Composite for Root Canal Irrigation.

The primary goals of endodontic therapy are to eliminate microbes and prevent reinfection. Persistent root canal infections and failure of root canal therapy are primarily attributed to the presence of bacteria, particularly E. faecalis. Chemical irrigants play a crucial role in complementing mechanical instrumentation in ensuring adequate disinfection. However, current techniques and available irrigants are limited in their ability to achieve optimal sterilization of the root canal system. In this study, we developed a novel material called La@PCDs by combining CQD-PVA and lanthanum for root canal irrigation. A one-pot hydrothermal method was used to prepare composites of lanthanum and CQD-PVA (La@PCDs). Scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy and the particle size were employed to characterize La@PCDs. ROS generation was evaluated by measuring the fluorescence intensity emitted at 525 nm from 2',7'-dichlorodihydrofluorescein diacetate (DCFH-DA). In vitro experiments were conducted to assess the effectiveness of the nanoparticles in combating Enterococcus faecalis and eradicating in situ biofilm eradication in root canal. Furthermore, cytotoxicity assessments were carried out to demonstrate the safety of La@PCDs. SEM and FTIR results showed that La@PCDs were successfully prepared and exhibiting a homogeneous size distribution and irregular morphology. ROS assessment demonstrated that La@PCDs have a synergistic effect, promoting the production of a large number of ROS. This effect only occurred under acidic PH conditions. The inherent acidity in the biofilm microenvironment can act as internal stimulus. In vitro experiments revealed superior antibacterial efficiency under acidic conditions without causing significant cytotoxicity compared to the commonly used NaClO irrigant. The biosafety of La@PCDs was confirmed. Compared to existing materials, these nanoparticles exhibit favorable antibacterial and anti-biofilm properties, along with improved biocompatibility. These findings emphasize the potential of the integrated La@PCDs as a promising option for enhancing root canal irrigation and disinfection.

Synthesis and Characterization of Synergetic Pd/MoO3–rGO Hybrid Material as Efficient Electrode for Supercapacitor Application

In this work, study synthesized Pd–rGO and Pd/MoO3–rGO nanocomposites via a one-pot hydrothermal method, serving as efficient electrodes for supercapacitor applications. Various analytical techniques, including XRD, XPS, HRTEM, BET, and Raman spectroscopy, were employed to characterize the structural, morphological, and physiochemical properties to assess the electrochemical supercapacitor performance of nanocomposite materials. The analyses confirmed that the charge transfer mechanism between the MoO3-NR with Pd-rGO in Pd/MoO3–rGO samples has significantly improved the electrochemical performance of Pd/MoO3–rGO by 2.7 times compared to Pd-rGO sample (105.00 F/g at 0.5 A/g). Remarkably, the Pd/MoO3–rGO hybrid material exhibited excellent electrochemical activity, boosting a specific capacitance of 291.50 F/g at a current density of 0.5 A/g, accompanied by energy density and power density values of 18.06 Wh/kg and 250.00 W/kg, respectively. Furthermore, it demonstrated noteworthy stability over prolonged usage, retaining 88.46% of its capacity after 1,000 cycles at a constant current density of 1.0 A/g. These findings underscore the promising potential of the Pd/MoO3–rGO nanocomposite as a highly effective electrode material for supercapacitors.

Molten salts assisted one-pot synthesis of hollow transition metal carbides

Molten salts assisted one-pot synthesis of hollow transition metal carbides

Cysteamine functionalized gold nanoparticles exhibit high efficiency delivery of genetic materials in embryonic stem cells majorly via clathrin mediated endocytosis

Efficient and safe gene delivery is vital for genetic manipulation of stem cells for regenerative medicine. Gold nanoparticles have been used for various biomedical applications in the past, and are currently being researched as transfection agents. In this study, we report a simple one-pot synthesis of positively charged gold nanoparticles functionalized with cysteamine. The nanoparticles exhibit no cytotoxicity and can bind to both plasmid DNA (pDNA) as well as small interference RNA (siRNA). We observed that a five fold lower concentration of pDNA was sufficient for achieving comparable overexpression as that of a commercial transfection agent. We also observed that about 70 % transient silencing of the target gene was achieved with only 25 nM siRNA delivered by our nano-vehicle. To better understand the fate of the nanoparticle, we attempted to identify its uptake mechanism. The results indicate that while all the mechanisms contribute to the uptake, the clathrin-dependent pathway plays a major role. This is the first study on understanding the mechanism of uptake of CA-AuNPs conjugated to pDNA by embryonic stem cells. This is also the first study, where a successful transfection using gold based nanoparticles has been achieved in ESCs at a concentration as low as 0.5 µg/ml for pDNA and 25ƞM siRNA.

One-Pot Synthesis of Mixed-Phase MoVTeNbOx Catalysts for Selective Oxidation of Propane to Acrylic Acid.

One-pot hydrothermal synthesis assisted by sodium citrate and citric acid is developed to fabricate mixed-phased MoVTeNbOx catalysts with different phase compositions for selective oxidation of propane to acrylic acid. Structures of various catalysts are comprehensively characterized. Interfacial interactions occur among the M1 and M2 phases of mixed-phase MoVTeNbOx catalysts to exert synergistic effects on the selective production of acrylic acid. Various mixed-phase MoVTeNbOx catalysts exhibit the same type of active site on the M1-phase component, with a significantly enhanced ability to adsorb and activate propane. The propane conversion increases linearly with the density of surface site for propane adsorption, while the propene selectivity increases linearly with the density of surface site for propene adsorption. Among the synthesized catalysts, a MoVTeNbOx catalyst composed of 35.3 wt % M1 phase, 19.2 wt % M2 phase, and 45.7 wt % amorphous phase exhibits the largest density of active site and consequently the best catalytic performance with 38.9% propane conversion and 71.2% acrylic acid selectivity at 380 °C.

Disparity between rate and selectivity in the controlled synthesis of gradient conjugated copolymers

In this report, a one-pot synthesis of gradient copolymers is attempted employing Kumada catalyst transfer condensative polymerization (KCTCP). The hypothesis that a more reactive monomer is preferentially being built into the chain at the beginning, while the slower reacting monomer is only being built into the chain at the end due to it being in excess, is investigated. The monomer rate constants are influenced by the usage of differently sized sidechains (octyl versus 3-octyldodecyl) and nucleophilicity of the monomers (thiophene versus selenophene). Nonetheless, while the rate constants differ by a factor 2, no selectivity is obtained. The cause thereof is further investigated by increasing the sterical crowdedness around the catalyst-complex by employing a 4-substituted monomer, the polymerization of which also gave rise to random copolymers. Accompanied by density functional theory calculations of the geometry and Gibbs free energy, it is concluded that the distance between the nickel catalyst and the polymer chain is much smaller compared to the distance between the catalyst and the incoming monomer. This results in different polymerization rates (depending on the polymer-nickel complex), while having no selectivity for one incoming monomer over the other.

One-pot synthesis of non-canonical ribonucleosides and their precursors from aldehydes and ammonia under prebiotic Earth conditions

The formation of polymers that can hold gene information and work as catalysts is a crucial step for the origin of life. The discovery of catalytic RNA (i.e., ribozyme) supports the hypothesis that RNA might have served these functions at the early stage of life on the Earth. Given this, the spontaneous formation of RNA monomers (i.e., ribonucleotides) and their polymerization on Hadean Earth are essential steps for the origin of life. Previous experiments have investigated the chemical reactions that allow the formation of ribonucleotides and their components. These works have revealed the required molecules to form biological ribonucleotides (i.e., canonical ribonucleotides). Based on geochemical perspectives, abundantly available reactive molecules spontaneously react with each other to provide abundant products. Aldehydes and ammonia are reactive molecules assumed to have been present in considerable amounts on Hadean Earth. However, little is understood about whether or not nucleotides and their components were formed from these molecules under prebiotic conditions. We investigated the incubation products of alkaline aqueous solutions of aldehydes and ammonia. The product solution contained sugars (including ribose), various imidazole derivatives, and ribosyl imidazole (i.e., imidazole ribonucleoside). Ribosyl imidazole is formed via ribosyl amine, which reveals a new reaction pathway for prebiotic ribonucleoside synthesis. The imidazole ribonucleoside was then phosphorylated to imidazole ribonucleotide via a simple dry-down reaction with phosphate. Borate ion improved the reaction yields of these nucleosides and nucleotides. Because all the reactants were available on prebiotic Earth and the reactions progressed spontaneously, imidazole ribonucleotides could have accumulated in prebiotic environments. The experimental simplicity of the present reaction suggests that imidazoles were more abundant than canonical nucleobases on the prebiotic Earth. This further implies that prebiotic oligonucleotides contained imidazole bases in addition to the canonical nucleobases. The improvement of the reaction yields by borate indicates that borate-rich environments were conducive places for the formation and accumulation of non-canonical nucleosides and nucleotides. Such environments could have facilitated the formation of primordial ribonucleic acids on Hadean Earth.

Ionic liquid promoted facile one-pot synthesis of phenothiazine-thiazolidin-4-ones as potent antitubercular agents via mycobacterial ATP synthase inhibition

The mycobacterial ATP synthase is responsible for the optimal growth, metabolism and viability of mycobacteria, establishing it as a validated target for the development of anti-TB therapeutics. Herein, we report the facile and efficient one-pot three component synthesis of 2-(10H-phenothiazin-3-yl)-3-substituted thiazolidin-4-one derivatives by using ionic liquid, 1-butyl-3-methylimidazolium bromide [Bmim]Br and their inhibitory potency against mycobacterium tuberculosis H37Rv strain (ATCC-27294). Compound T27 exhibited the highest inhibition activity with an MIC of 0.78 μg/mL, which is twofold and fourfold superior (in terms of the MIC values) to the standard first-line TB drugs isoniazid (MIC: 1.56 μg/mL) and pyrazinamide (MIC: 3.12 μg/mL) respectively. Two other compounds (T25 and T30) are equipotent as the isoniazid. The SAR studies revealed that insertion of 1,2,3-traizole and thiozolidine-2-one rings enhance the anti-TB activity in most of the tested compounds. Also, compound T27 was screened for mycobacterial ATP synthase inhibition activity and it exhibited an IC50 of 0.735 µM in M. smegmatis IMVs. Further, toxicity evaluation against VERO cell lines confirmed null cytotoxicity (selectivity index > 70) of the potent analogues. The title compounds are highly specific towards to the M. tb strain, i.e., most of the compounds exhibited moderate inhibitory potency against the tested bacterial strains (MIC ≥ 6.25 μg/mL). In addition, molecular docking was employed against the active site of the ATP synthase enzyme to validate the binding mechanism and in vitro activity profile of the phenothiazine derivatives. Furthermore, in silico ADME and pharmacokinetic parameters’ prediction indicated good oral bioavailability.

One-pot synthesis of tricyclic pyrano[3.2-c]chromene derivatives and their evaluation through in vitro immunomodulatory activity against T cells; Molecular docking investigations and ADME-Tox prediction studies

The aim of this work is the in vitro determination of the immunomodulation effect of pyrano[3,2-c]chromenes on the proliferation of T lymphocyts. These tricyclic heterocycles were prepared at room temperature via a one-pot, three-component condensation reaction involving 4-hydroxy-2H-chromen-2-one, aromatic aldehydes, and malononitrile, using morpholine as a catalyst in a 1:1 ethanol/water mixture. This multicomponent reaction affords the product in high yields, in accordance with the criteria of green chemistry. The structure elucidation was accomplished by spectral data, IR, NMR (1H, 13C, 2D). We determined the in vitro effects of 2-amino-4-(3-hydroxy-5-methoxyphenyl)-5-oxo-4H,5H-pyrano[3,2-c]chromene-3-carbonitrile (AC09) the 2-amino-5-oxo-4-(thiophen-2-yl)-4H,5H-pyrano[3,2-c]chromene-3-carbonitrile (AC11) derivatives, on the proliferative responses of human T lymphocyts cells, cytokine secretion and intracellular redox status. The study revealed that compounds AC09 and AC11 are efficient immunostimulants in a dose-dependent manner.Human lymphocytes were less sensitive to AC11 at high concentrations compared to the potency of AC09. Human lymphocyte IL-2, IFNγ and IL-4 secretions were significantly enhanced by those pyrano[3,2-c]chromenes derivatives in a dose-dependent manner. The levels of intracellular lymphocytes glutathione (GSH), were unaffected by AC09 and AC11 at any concentrations. AC09 and AC11 induce a significant increase in hydroperoxide and carbonyl protein contents at high concentrations. Conversely, a computational study using molecular modelling revealed that compounds AC09 and AC11 exhibit a strong affinity for the active site residues of Interferon-γ (IFN-γ; PDB ID: 6E3K) target. This is confirmed by the low score energy value and the formation of different types of interactions such as: hydrogen bonds, hydrophobic interactions, and van der Waals forces. Moreover, all Drug likeness's rules were validated, and no toxicity is presented by these compounds. Finally, in vitro studies, molecular docking techniques and ADME-T (Absorption, Distribution, Metabolism, Excretion and Toxicity) evaluations were successfully conducted, aiding in the identification of new IFN-γ target inhibitors. A comparative analysis /or studies was then carried out to highlight the complementary effects of the two approaches.

One-pot synthesis of graphene nanosheets‑nickel cobalt LDHs nanocomposite for electrocatalysis of oxygen evolution reaction

Oxygen evolution reaction (OER) is known as a bottleneck for the overall water-splitting process due to its slow kinetics. In this regard, constructing a high-performance, cost-effective electrode material may act as a game changer. Here, a 2D/2D nanocomposite has prepared out of graphene nanosheets and nickel‑cobalt layered double hydroxide (NiCo LDH) by a simple solvothermal method. The 2D flower-like structures of NiCo LDH attached to graphene nanosheets have observed in field-emission scanning (FE-SEM) and transmission (TEM) electron microscopy images. The X-ray diffraction (XRD) patterns have revealed the formation of Ni(OH)2 and Co(OH)2 lattices along with hexagonal graphene crystals. X-ray energy dispersive spectroscopy (EDS) has noted the 2.2:1 ratio of nickel to cobalt in the graphene/NiCo LDH nanocomposite. X-ray elemental maps have shown the uniform distribution of elements in the sample, and the corresponding functional groups have observed in the Fourier-transform infrared (FTIR) and Raman spectra. X-ray photoelectron spectroscopy (XPS) has determined the coexistence of divalent and trivalent metals in the nanocomposite. The N2 adsorption-desorption study has shown signs of slit-shaped ion-accessible micro and mesopores with high specific surface area for the nanocomposite. It has benefited the ion diffusion process during the exposure of the modified electrode to the electrolyte. The graphene/NiCo LDH nanocomposite has provided the onset potential of 1.56 V, overpotential of 338 mV at 10 mA cm−2, Tafel slope of 69 mV dec−1, charge-transfer resistance (Rct) of 27 Ω, double layer capacitance (Cdl) of 24 μF, electrochemically surface area (ECSA) of 0.6 cm2, and roughness factor (RF) of 20. The electrode has maintained 98.3 % of its initial signal after 10 h continuous measurement at OER potential. This electrocatalytic activity refers to the sheet-like morphology, effective hydroxide ion transfer through interlayer spaces, enhanced conductivity, and high chemical stability achieved by a constructive synergy between graphene nanosheets and NiCo LDH.

One-pot synthesis of hydroxypropyl methylcellulose-based gel polymer electrolytes for high-performance supercapacitors

The electrolyte is a crucial component that significantly affects the electrochemical performance of supercapacitors. The hydroxypropyl methylcellulose (HPMC)-based gel polymer electrolyte (GPE) with high operating voltage was synthesized via an innovative “one-pot” method in this study, and the impacts of organic solvent/water ratio and LiNO3 concentration on gelation and conductivity of the GPE were investigated systematically. Under the optimal condition with a DMF/water ratio of 10:0 and the incorporation of 7 % LiNO3, the ionic conductivity reached 1.06 S m−1. Integrated into symmetric supercapacitors, the HPMC-based GPE demonstrated an expanded electrochemical window of 2.7 V. It also possessed a specific capacitance of 115.8 F g−1 at 1.0 A g−1, an energy density of 29.31 Wh kg−1, and outstanding cyclic stability, retaining 86 % of its initial capacitance after 2000 cycles. Through cyclic stability tests under pressure conditions, the assembled flexible supercapacitors were able to maintain capacitance retention of 60 % and coulombic efficiency of 97 %. This work offers a streamlined synthesis for HPMC-based GPE with superior electrochemical properties, which exhibits its potential in advancing supercapacitor technology for flexible electronics.

One-pot Synthesis of 2,3-disubstituted-4(3H)-quinazolinone from o-aminobenzoic Acid and DMF Derivatives using Imidazole Hydrochloride as a Promoter.

As a novel and environmentally friendly Brönsted acid, imidazole hydrochloride was used to promote the synthesis of 2,3-disubstituted-4(3H)-quinazolinone from o-aminobenzoic acid and DMF derivatives. The essence of this reaction is a multicomponent reaction, which constructs multiple chemical bonds between different components through the transamidation of imidazole hydrochloride. This protocol showed a wide range of functional group tolerance, and a series of quinazolinones were synthesized in low to moderate yields without metal catalysts, oxidants or other additives.

Efficient synthesis of novel phenanthroline-dimedone derivatives using Pd@HQBI-SPION as a versatile palladium-immobilized catalyst

This paper presents the synthesis and application of a novel catalyst for carbon–carbon bond formations, comprising palladium immobilized on 2-(5-hydroxyquinolin-8-yl)-1H-benzo[d]imidazole-5-carboxylic acid modified superparamagnetic iron oxide nanoparticles (Pd@HQBI-SPION). The synthesis involved the attachment of HQBI ligands to SPION using APTES, followed by the immobilization of palladium. Characterization techniques, including FTIR, TEM, and magnetic measurements, confirmed the successful synthesis and structural integrity of Pd@HQBI-SPION. The catalytic activity of Pd@HQBI-SPION was evaluated in various carbon–carbon bond formation reactions, demonstrating high efficiency and reusability. 8 different derivatives bearing several electron withdrawing and electron donating functionalities were used as starting materials and the products were obtained in high isolated yields (75–97%). The catalyst exhibited excellent performance in one-pot synthesis of phenanthroline-dimedone polycyclic derivatives via C-alkylation followed by intramolecular O-alkylation of phenanthroline with dimedone. The products are obtained in high to excellent yields is described. This protocol presents a highly selective synthetic method for the construction of polycyclic aromatic compounds containing nitrogen and oxygen atoms.

A green chemistry approach for one-pot synthesis and antibacterial studies of 2,3′-bi-indole derivatives using Brønsted acid ionic liquid as an organocatalyst

A green chemistry approach for one-pot synthesis and antibacterial studies of 2,3′-bi-indole derivatives using Brønsted acid ionic liquid as an organocatalyst

Design and Synthesis of Novel Heterocycles Utilizing 4,6-Dimethyl-1- ((4-methylthiazol-2-yl)amino)-2-oxo-1,2-dihydropyridine-3-carbonitrile

Abstract: Novel hydrazones 4, 5, and oxime 6 were produced from the reaction of ketone 3 with hydrazine, phenylhydrazine, and hydroxylamine HCl, respectively. One pot multicomponent reaction of chalcones 7a-c, 3-(1H-indol-3-yl)-3-oxopropanenitrile 8, and ammonium acetate in MeOH at reflux temperature gave 2-(1H-indol-3-yl)-nicotinonitrile derivatives 10-12. Additionally, a one-pot reaction of chalcone 7a, malononitrile or ethyl cyanoacetate, and ammonium acetate in AcOH at reflux temperature afforded 6-aminopyridine derivatives 13 and 14, respectively.

Electrochemical-promoted Mannich-type three-component reaction of benzo-fused cyclic amides using methanol as C1 source instead of formaldehyde

The three-component N-Mannich reaction is provided in an electrochemical variant. The corresponding N-Mannich base products were obtained by the one-pot method of benzo-fused cyclic amides with secondary amines under a small current of 3 mA using methanol as the carbon source. The reaction is simple to carry out (room temperature and air environment) and requires no supporting electrolytes, using TEMPO as the oxidizing agent. The substrate scope is wide, and the yield is good (39 cases, up to 99 %). CV experiments show that secondary amines are oxidized first at the anode. Moreover, this reaction can be scaled up to the grams.

Preparation of carboxylated-silk nanofibers by the one-pot method of maleic acid hydrolysis

Preparation of carboxylated-silk nanofibers by the one-pot method of maleic acid hydrolysis

A facile one-pot synthesis of hierarchical porous carbon for supercapacitor electrodes

This study presents a facile, environmentally friendly approach to fabricate hierarchical porous carbon for supercapacitor electrodes. The one-pot synthesis of PFO/silica/PTFE via co-pyrolysis generates ideal hierarchical porous carbon. Compared with traditional methods, this method eliminates toxic solvents and complex cleaning steps. PPC-2 obtained under the optimized activation time has the highest specific surface area (2657 m2 g−1) and a remarkable total pore volume (2.96 cm3 g−1). These properties result in a remarkable specific capacitance of 335.9–210.8 F g−1 at current densities of 0.5–10 A g−1 in KOH electrolyte. The electrochemical performance of the PPC-2 electrode in a symmetric supercapacitor device was measured in aqueous (6 M KOH) and ionic liquid (EMIM-TFSI) electrolytes. In EMIM-TFSI, PPC-2//PPC-2 provides an energy density of 48.5 Wh/kg even at a power density of 750 W kg−1. This facile one-pot synthesis method offers a sustainable and scalable approach to produce high-performance hierarchical porous carbon for supercapacitor applications.