Efficient Method For Synthesis Research Articles

Enhancing Stability of Microwave-Synthesized Cs2SnxTi1-xBr6 Perovskite by Cation Mixing.

The double-perovskite material Cs2TiBr6 shows excellent photovoltaic potential, making it a promising alternative to lead-based materials. However, its high susceptibility to degradation in air has raised concerns about its practical application. This study introduces an interesting synthesis approach that significantly enhances the stability of Cs2TiBr6 powder. We implemented a gradual cation exchange process by substituting Ti4+ with Sn4+ in the efficient microwave-assisted synthesis method, developing a double perovskite Cs2SnxTi1-xBr6 type. A systematic study of increasing concentration of Sn4+ in Cs2TiBr6 perovskite has been performed to analyze the effect of Sn-doping degree on the chemical and thermal stability of the material and the optical features in both nitrogen and ambient atmospheres, significantly increasing the stability of the material in the air for over a week. Furthermore, introducing Sn4+ results in a more uniform polygonal crystal morphology of the powders and a slight band gap broadening. We show that microwave-assisted synthesis is highly efficient and cost-effective in producing more sustainable lead-free perovskite materials with enhanced stability and desirable electrical characteristics. This work suggests a promising method for synthesizing perovskite materials, opening new routes for scientific research and applications.

Three-dimensional nanocomposites derived from combined metal organic frameworks doped with Ce, La, and Cu as a bifunctional electrocatalyst for supercapacitors and oxygen reduction reaction

Fabrication of a nanocomposite with a low-cost and efficient synthesis method instead of using electrocatalysts based on platinum metal has become one of the main challenges in energy storage devices and fuel cells. In this regard, a bifunctional electrocatalyst for supercapacitors and oxygen reduction reaction is fabricated and tested. The novelty of this study is the synthesis method and enhancement of the electrochemical characteristics of synthesized electrocatalysts. The core-shell method is used for the electrocatalyst's synthesis which uses Zeolitic Imidazolate Framework (ZIF)-8, ZIF-67, and Material Institute Lavoisiers (MIL)-101 for the fabrication of three types of electrocatalysts. In the following, to increase the characteristics such as conductivity and stability, doping of Copper (Cu), Cerium (Ce), and Lanthanum (La) are added to the nanocomposites. The Co@NC, CoZn@NC, and CoZn@FeNC prepared electrocatalysts are obtained from the pyrolyze process of La/ZIF-67, CeCu/ZIF-8@ La/ZIF-67, MIL-101@CeCu/ZIF-8/La/ZIF-67. The results indicated that the CoZn@NC electrocatalyst has the best performance in the oxygen reduction reaction (ORR) with an onset potential of 0.062 (V vs Ag/AgCl) and current density of −12.97 (mA/cm2) at a constant voltage of −1 V. Furthermore, the electron transfer number of CoZn@NC electrocatalyst for ORR was 3.64. The conducted Galvanostatic Charge-Discharge (GCD) tests demonstrated that the CoZn@NC electrode has the highest capacitance of 271.14 F/g. The outcomes showed that by the core-shell method, various properties of nanocomposites can be utilized to solve the weaknesses of catalysts by using proper metals. Moreover, the presence of Cu2+,Ce3+,La3+ improve the structural defects in the carbon matrix, the stability based on the chronoamperometry results, and the mass transfer. The study provides a perspective for future researches to fill the research gaps to obtain the new supercapacitors utilize on a large scale in the electronics industry.

Facile Access to Benz[c,d]indolium-containing Dyes: C-N and C-C Bond Formation and Their Photophysical Properties

This work explores an efficient synthesis method for 1,8-Np derivatives, focusing specifically on the relatively inactive site (site II) of 1,8-Np, as well as the low-activity NH site present in secondary amine compounds. Derivatives Np-A-1∼9 are synthesized by forming C-N bonds with POCl3 acting as the activating reagent, achieving good yields (30∼62%). Next, substrate expansion on 1,8-Np proceed with other secondary amine compounds. Np-B and C are synthesized by forming C-N bonds, however, Np-D-1, 2 are synthesized by forming C-C bonds. This is a mild approach for forming C-N and C-C bonds, which is beneficial for the preparation of near-infrared (NIR) fluorescent dyes. Optical properties in solvents are discussed for Np-A∼D. This system shows large Stokes shifts (4513∼9105cm-1). The AIE phenomenon and solid-state emission properties are observed in Np-A-1∼9, which exhibit strong AIE phenomena, featuring 1.3 to 7.1-fold fluorescence intensity enhancement and solid fluorescence quantum yield ranging from 6.08 to 15.27%. The substitution on the indole unit is beneficial for enhancing the AIE effect and increasing the solid fluorescence quantum yield. Single crystal analysis and DFT calculation further elucidate the structures and the optical properties.

Enhanced super capacitance performance of V₂O₅·nH₂O/g-C₃N₄ nanocomposites: Synthesis, characterizations, and electrochemical properties

The primary problem addressed in this study is to enhance the performance of supercapacitor electrode materials by developing a cost-effective, and efficient synthesis method for nanocomposites with high capacitance. Hence, in this study, we report the synthesis of V2O5·nH2O/g-C3N4 nanocomposites using a cost-effective hydrothermal method, resulting in four distinct samples: pristine V2O5·nH2O nanoribbons (VO) and three composites with varying amounts of g-C3N4 (10, 20, and 30 mg), labelled as VCN1, VCN2, and VCN3. Structural, morphological, optical, and electrochemical characterizations were conducted to assess their potential as supercapacitor electrode materials. Electrochemical analysis, including cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD), confirmed pseudocapacitance behavior in all samples. VCN1, containing 10 mg of g-C3N4 in V2O5·nH2O matrix, exhibited the highest specific capacitance of 230 F/g at a scan rate of 10 mV/s in a 3M KOH electrolyte. This enhancement in capacitance is attributed to the added g-C3N4, which increases active sites, as confirmed by Electrochemically Active Surface Area (EASA) measurements. Additionally, electrochemical impedance spectroscopy (EIS) supported VCN1's superior performance, identifying it as a promising, cost-effective electrode material for super capacitor applications.

An Efficient Method for the Selective Syntheses of Sodium Telluride and Symmetrical Diorganyl Tellurides and the Investigation of Reaction Pathways.

Studies on organotellurium compounds have not been extensively conducted due to a lack of tolerable synthetic methods, difficult isolation processes, and their chemical instabilities. Overcoming these hurdles, we developed an efficient and mild method for the selective synthesis of symmetrical diorganyl tellurides 1, a representative class of organotellurium compounds, using a proper reducing reagent. The reaction condition was optimized for the selective formation of 1 by forming the telluride dianion (Te2-) using a reducing reagent, sodium borohydride (NaBH4), and then followed by the addition of organyl halides. The optimized reaction condition was as follows: (1) Te (1.0 eq), NaBH4 (2.5 eq) in DMF for 1 h at 80 °C; (2) organyl halides (2.0 eq) for 3-5 h at 25-153 °C. Using this condition, 18 various diorganyl tellurides 1 were selectively and efficiently synthesized in reasonable yields (37-93%). The reaction pathways for the formation of diorganyl tellurides 1 were also investigated. Consequently, we established a practical and efficient method for the selective synthesis of diorganyl tellurides 1 as a representative class of organotellurium compounds.

Eco-friendly synthesis and high-efficiency adsorption of potassium permanganate using a magnetic hydrochar composite derived from Calotropis procera

Water pollution poses significant health and environmental risks, impacting ecosystems and human health. This study investigates the removal of potassium permanganate (KMnO4) from water using a magnetic hydrochar composite (HTCNP) synthesized from Calotropis procera (CP) leaves through a single-step hydrothermal carbonization process. This eco-friendly and efficient synthesis method provides an advantageous alternative to traditional multi-step processes. Structural analysis confirmed the composite’s porous structure and functional groups that contribute to effective adsorption. Under optimal conditions (pH 7, adsorbent dose of 1 g/L, contact time of 60 minutes, and temperature of 298 K), HTCNP achieved a maximum adsorption capacity of 388.09 mg/g. Adsorption kinetics followed a pseudo-second-order model, and the adsorption behavior aligned with the Freundlich isotherm, indicating multilayer adsorption on a heterogeneous surface. Furthermore, the HTCNP composite demonstrated good reusability over five cycles, maintaining high removal efficiency, and effectively removed KMnO4 from real wastewater samples. These findings highlight the potential of HTCNP as an efficient, sustainable, and practical adsorbent for water purification applications, contributing to environmental protection and public health improvement.

Enantioselective synthesis of inherently chiral sulfur-containing calix[4]arenes via chiral sulfide catalyzed desymmetrizing aromatic sulfenylation

Inherently chiral calixarenes hold great potential for applications in chiral recognition, sensing, and asymmetric catalysis due to their unique structures. However, due to their special structures and relatively large sizes, the catalytic asymmetric synthesis of inherently chiral calixarenes is challenging with very limited examples available. Here, we present an efficient method for the enantioselective synthesis of inherently chiral sulfur-containing calix[4]arenes through the desymmetrizing electrophilic sulfenylation of calix[4]arenes. This catalytic asymmetric reaction is enabled by a chiral 1,1’-binaphthyl-2,2’-diamine-derived sulfide catalyst and hexafluoroisopropanol. Various inherently chiral sulfur-containing calix[4]arenes are obtained in moderate to excellent yields with high enantioselectivities. Control experiments indicate that the thermodynamically favored C-SAr product is formed from the kinetically favored N-SAr product and the combination of the chiral sulfide catalyst and hexafluoroisopropanol is crucially important for both enantioselectivity and reactivity.

Recent Advances in Electrocatalytic C-N Coupling for Urea Synthesis.

Urea, one of the most widely used nitrogen-containing fertilizers globally, is essential for sustainable agriculture. Improving its production is crucial for meeting the increasing demand for fertilizers. Electrocatalytic co-reduction of CO₂ and nitrogenous compounds (NO₂-/NO₃-) has emerged as a promising strategy for green and energy-efficient urea synthesis. However, challenges such as slow reaction kinetics and complex multi-step electron transfers have hindered the development of efficient urea synthesis methods. This review explores recent advances in the electrocatalytic C-N coupling process, focusing on bimetallic catalysts, metal oxide/hydroxide catalysts, and carbon-based catalysts. The review also discusses the future prospects of designing effective catalysts for electrocatalytic C-N coupling to improve urea synthesis.

Preparation of Lipid–Polymer Conjugates by Photoiniferter Polymerization and Application to Cell Surface Modification

ABSTRACTThe growing demand for lipid–polymer conjugates (LPCs) in biomedicine highlights the need for efficient synthesis methods. This study presents a novel Y‐type photoiniferter reagent (Lipid‐PIT) with a diethyldithiocarbamate group and a diacylglycerol group. Lipid‐PIT efficiently initiated the polymerization of vinyl monomers such as oligo(ethylene glycol) methacrylate (OEGMA), N,N‐dimethylacrylamide (DMA), tert‐butyl acrylate (tBA), and n‐butyl acrylate (nBA) under UV irradiation at room temperature, yielding LPCs. Proton NMR confirmed the presence of diethyldithiocarbamate and diacylglycerol moieties at the chain ends. The polymerization kinetics of DMA showed a linear increase in molecular weight (Mn) with time, with a polydispersity (Đ) below 1.50, demonstrating high controllability. Moreover, Lipid‐PIT allows for the creation of block copolymers via secondary chain extension. In vitro assays revealed that LPCs synthesized from OEGMA monomers successfully modified L929 and HeLa cell surfaces and exhibited good biocompatibility. This study offers a rapid, efficient method for LPC synthesis with promising biomedical applications.

Divergent Regioselective Synthesis of Functionalized 1,2,3-1H-Triazoles from Nitriles and Arylazides Under Metal-Free and/or Solvent-Free Conditions.

Highly selective and divergent syntheses, which are crucial in both organic synthesis and medicinal chemistry, involve significant advancements in compound accessibility. By modifying α-cyano esters into α-cyano ketones, the synthesis pathway broadens to include a diverse range of 4-CN, 5-amino, and 5-arylamino derivatives of 1,2,3-triazoles, which are achieved notably through the Dimroth rearrangement. This versatility extends further with the potential for a triple cascade reaction, leading to the production of carboximidamide compounds, which are facilitated by the Cornforth rearrangement. Advancements in compound accessibility not only expand the repertoire of synthesized molecules but also open new avenues for potential pharmacological agents. Building on these findings, we have developed an innovative and efficient method for the divergent synthesis of functionalized 1,2,3-triazoles. This method strategically utilizes α-cyanocarbonyls and arylazides by harnessing their reactivity and compatibility to orchestrate a variety of molecular transformations. By optimizing these substrates, our goal is to simplify synthetic routes, improve product yields, and accelerate the discovery and development of new chemical entities with promising biological activities.

Asymmetric Synthesis of Chiral Calix[4]arenes with Both Inherent and Axial Chirality via Cobalt-Catalyzed Enantioselective Intermolecular C-H Annulation.

Inherently chiral calixarenes have garnered significant attention due to their distinctive properties, yet the development of efficient catalytic asymmetric synthesis methods remains a critical challenge. Herein, we report the asymmetric synthesis of calix[4]arenes featuring inherent or both inherent and axial chirality via a cobalt-catalyzed C-H activation/annulation strategy in high yield with excellent enantio- and diastereoselectivity (up to >99 % ee and >20 : 1 dr). Electrooxidation was also suitable for this transformation to obviate the sacrificial metal oxidants, underscoring the environmentally friendly potential of this approach. A key octahedral cobaltacycle intermediate was synthesized and characterized, providing valuable insights into the mode of enantio- and diastereocontrol of this protocol. Noteworthy photoluminescence quantum yields of up to 0.94 were measured, underscoring the potential of these compounds in the domain of organic fluorescent materials.

Asymmetric Synthesis of Chiral Calix[4]arenes with Both Inherent and Axial Chirality via Cobalt‐Catalyzed Enantioselective Intermolecular C−H Annulation

AbstractInherently chiral calixarenes have garnered significant attention due to their distinctive properties, yet the development of efficient catalytic asymmetric synthesis methods remains a critical challenge. Herein, we report the asymmetric synthesis of calix[4]arenes featuring inherent or both inherent and axial chirality via a cobalt‐catalyzed C−H activation/annulation strategy in high yield with excellent enantio‐ and diastereoselectivity (up to >99 % ee and >20 : 1 dr). Electrooxidation was also suitable for this transformation to obviate the sacrificial metal oxidants, underscoring the environmentally friendly potential of this approach. A key octahedral cobaltacycle intermediate was synthesized and characterized, providing valuable insights into the mode of enantio‐ and diastereocontrol of this protocol. Noteworthy photoluminescence quantum yields of up to 0.94 were measured, underscoring the potential of these compounds in the domain of organic fluorescent materials.

Direct Synthesis of Benzothiazoles and Benzoxazoles from Carboxylic Acids Utilizing (o-CF3PhO)3P as a Coupling Reagent.

A general and efficient method for the direct synthesis of benzothiazoles and benzoxazoles from carboxylic acids with 2-aminobenzenethiols or 2-aminophenols using (o-CF3PhO)3P as a simple coupling reagent has been developed. Diverse benzothiazoles and benzoxazoles were synthesized in moderate to excellent yields. And the gram-scale preparation of benzothiazole and benzoxazole also proceeded smoothly under the mild conditions. Moreover, a plausible reaction mechanism was discussed, with (o-CF3PhO)3P and its hydrolysis product (o-CF3PhO)2P(O)H contributing to the formation of the target products as an amide synthesis coupling agent and a cyclization reaction promoter, respectively.

Concise Synthesis and Biological Evaluation of the Pyrrolo[4,3,2-de]quinoline Core of the Lymphostin Family.

The efficient synthesis of the pyrrolo[4,3,2-de]quinoline core of the lymphostin family (compound 1) has been accomplished in 7 steps and 18.6% overall yield, providing an efficient method for the total synthesis and structural modification of the lymphostin family. Compound 1 showed potent inhibitory activities against PI3K/mTOR in the nanomolar range and activity against human colorectal cancer cell lines comparable to that of oxaliplatin, which could be recognized as a novel lead compound for cancer therapy.

Rapid and controllable microwave synthesis of nickel cobalt sulfide electrodes for high-performance asymmetric supercapacitors

The efficient and controllable synthesis method of high-performance energy storage electrode materials is crucial for advancing the development of energy storage technologies. Herein, by leveraging microwave heating technology in the sulfidation of nickel cobalt MOF, we effectively enhanced the efficiency of the synthesis process. Notably, sulfidation time emerged as a pivotal factor in tuning the crystalline phase structure and conductive properties of the material, leading to the successful development of NCS2 electrode material with a unique structure through optimized sulfidation conditions. Electrochemical performance tests of the NCS2 material revealed exceptional results; it exhibited a specific capacity of 1311 Fg[Formula: see text] at a current density of 1 Ag[Formula: see text] and retained 73.4% of its initial capacity when the current density increased to 10 Ag[Formula: see text], demonstrating outstanding rate performance. The composite NCS2//AC supercapacitor exhibits an energy density of 24.2 Whkg[Formula: see text] at power density of 800 Wkg[Formula: see text], even though after 1000 consecutive charge-discharge cycles, the capacity retention rate remained high at 77.1%, validating the exceptional stability and reliability of the NCS2 material during cycling. This work employs microwave sulfidation for the rapid and controlled synthesis of nickel cobalt sulfides, providing a green and efficient synthetic strategy for metal sulfide active materials.

High entropy 2D metals sulfides: Fast synthesis, exfoliation and electrochemical activity in overall water splitting at alkaline pH

Novel simple and efficient method for synthesis of 2D high entropy sulfides of iron group metals is described. The method utilizes inorganic salts as precursors and CS2 as a sulfurizing agent, which makes it possible to achieve high entropy composition through combination of freezing of the precursor solution, subsequent freeze-drying step, sulfurization, and exfoliation in liquid nitrogen. The created material was investigated as a catalyst for electrochemical water splitting at different pH. Measured overpotentials at 10 and 100 mA*cm−2 current densities for hydrogen evolution reaction (HER) were found to be 49 and 315 mV respectively, while for oxygen evolution reaction (OER) theoverpotentials required for reaching 10 and 100 mA*cm−2 current densities were 370 and 591 mV respectively, both in 1 M KOH solution. The Tafel slopes for HER were found to be 235, 105, and 111 mV/dec in basic, neutral, and acidic conditions, respectively, while only 63 mV/dec for OER in basic conditions. The calculated values of the turnover frequency were 0.62 s−1 for HER and 0.10 s−1 for OER. We also confirmed the key role of high entropy in the catalytic activity of the material by excluding individual elements from the composition of the HES.

Machine learning-assisted identification of potential cancer inhibitors: Multifunctional biomineralized CaCO3-polyethyleneimine nanoparticle carriers and their application in lung cancer therapy

Cancer, as a prevalent phenomenon among malignant tumors, has a late-stage diagnosis rate approaching half, significantly limiting treatment efficacy and imposing substantial physiological and psychological burdens on patients. Therefore, developing innovative therapeutic platforms that simultaneously optimize diagnostic accuracy, enhance therapeutic efficacy, and minimize side effects is a critical scientific challenge in the field of precision cancer medicine. In this study, we employed a simple and efficient one-pot synthesis method combined with polyethyleneimine (PEI)-mediated biomineralization technology to successfully prepare calcium carbonate-polyethyleneimine (CaCO3-PEI) composite nanoparticles. These nanoparticles exhibit high pH sensitivity and can rapidly degrade under the mildly acidic conditions that mimic the tumor microenvironment, providing potential for targeted tumor therapy. Subsequently, we encapsulated compound 1, which has potential for lung cancer treatment, within the CaCO3-PEI nanoparticles, successfully constructing the CaCO3-PEI@1 composite system. Structural analysis of this composite system was conducted through characterization techniques. In vitro cell experiments demonstrated that the CaCO3-PEI@1 composite system exhibited significant anticancer effects by effectively inhibiting cancer cell proliferation through the regulation of apoptosis-related protein Bax expression. This provides new insights and experimental evidence for the development of cancer treatment strategies. Based on the experiment and molecular docking identified activity against lung cancer, the compound 1 was used as the initiator for the machine learning model, and up to 10,000 episodes were generated, after thorough examination, it was found about two-thirds of the generated episodes were entirely different from each other, which demonstrated that the machine learning model was a powerful tool for designing of potential inhibitors against lung cancer.

Synergistic effect of SGO/Nickel cobalt sulfide nanocomposite on Ni-foam for supercapacitor performance with widened potential windows − A microwave-assisted synthesis

Designing of high-performance supercapacitors with superior energy storage capabilities is crucial for addressing the growing demand for sustainable energy solutions. In this study, we investigate the synergistic effect of a sulfonated graphene oxide (SGO) /nickel-cobalt sulfide (NiCoS) nanocomposite on Ni-foam for supercapacitor applications. The SGO/NiCoS nanocomposite exhibits improved electrochemical performance, including increased specific capacitance, enhanced rate capability, and widened operating potential windows. The material exhibits a high energy density of 117.76 Wh/kg and a power density of 503.24 W/kg. The ASC also showed superior electrochemical stability, retaining 90 % of its coulombic efficiency after 10,000 cycles. The combination of NiCoS and SGO on Ni-foam significantly augments energy and power density, making it an attractive material for advanced supercapacitors. The microwave-assisted synthesis technique employed in this study enables rapid and uniform heating, reducing reaction times and improving selectivity. This work demonstrates the potential of SGO/ NiCoS nanocomposites on Ni-foam for supercapacitors, highlighting the benefits of synergistic material combinations and efficient synthesis methods.

One‐Pot Synthesis of Fused Isoxazolo[4′,5′:3,4]pyrrolo[2,1‐b] Quinazolines as Potent EGFR Targeting Anticancer Agents

AbstractIn response to the need for scaffolds for medical applications, synthetic chemists have developed simple and efficient methods for optimal synthesis. To investigate the synthesis of fused isoxazoles in the presence of [3+2] cycloaddition followed by C−N bond formation reaction between 3‐((4‐iodo‐3‐phenylisoxazol‐5‐yl)methyl)quinazolin‐4(3H)‐one and various nitrile oxides was carried out by previously reported conditions. The cancer activities of the synthesized compounds were then tested in vitro against two cancer cell lines, MCF‐7 and A‐549. Three of the compounds, 3‐(3,5‐dichlorophenyl) isoxazolo[4′,5′:3,4]pyrrolo[2,1‐b]quinazolin‐9(11H)‐one, 3‐(4‐fluorophenyl)isoxazolo[4′,5′:3,4]pyrrolo[2,1‐b]quinazolin‐9(11H)‐one, and 3‐(4‐(trifluoromethyl)phenyl)isoxazolo[4′,5′:3,4] pyrrolo[2,1‐b] quinazolin‐9(11H)‐one has shown superior activity against the non‐small‐cell lung cancer cell line (A‐549) than the standards 5‐fluorouracil and erlotinib. Later, in vitro EGFR results revealed that a more potent compound was more effective than the conventional medicine, erlotinib. In silico investigations of more potent compounds and erlotinib on the EGFR protein indicated that more potent compounds had comparable binding energies and inhibition constants to erlotinib.

Influence of various concentrations of chloroauric acid on the fabrication of gold nanoparticles: Green synthesis using Elaeis guineensis Jacq leaf extract and characterizations

This work studies a green method for synthesizing gold nanoparticles (AuNPs) using Elaeis Guineensis Jacq. (oil palm) leaf extract (EGE) using a precursor of chloroauric acid (HAuCl4). The influence of various HAuCl4 concentrations on the formation of AuNPs by the green method was investigated. Characterization methods were employed to analyze the optical properties, size, shape, structure, and SERS applicability of the AuNPs. The findings suggest that EGE contains biomolecules like flavonoids and phenols, which fulfil the roles of reducing and capping agents during the synthesis of AuNPs. The AuNPs were fabricated spectroscopically at around 525 nm and validated by UV–Vis spectrophotometer. FT-IR result presents that the stretching vibrations of the hydroxyl (O–H) molecule are indicated by the large peak absorption at 3336 cm−1, demonstrating the O–H functional groups in the derivatives of phenols. The carbonyl (CO) stretching vibrations, generated by the carboxylic acid in flavonoids and phenols, exhibited a robust absorption at 1602 cm−1. An optimal HAuCl4 concentration of 0.69 mM resulted in AuNPs with uniform spherical morphology and a 10–30 nm size range confirmed by TEM analysis. This concentration also led to the strongest Raman intensity, indicating the potential of these biogenic AuNPs for SERS applications. Overall, the study demonstrates a sustainable and efficient method for AuNP synthesis using a readily available plant extract, paving the way for their use in advanced sensing technologies.