Simple Route Research Articles (Page 1)

A highly efficient and simple route for the synthesis of alkynyl sulfides has been developed by copper catalyzing the cross-coupling reaction of alkynyl halides/terminal alkynes with arylthioaluminum reagents. Various alkynyl sulfides can be obtained with 12-96% yields from the cross-coupling between alkynyl halides and arylthioaluminum reagents using 5 mol % Cu2O/10 mol % TFP (tri(2-furanyl)phosphine) as the catalyst at 100 °C for 1 h. In the one-pot step-by-step method, various alkynyl sulfides can be obtained with 5-93% yields from the cross-coupling between terminal alkynes and arylthioaluminum reagents using 5 mol % Cu(OAc)2/10 mol % DPPY (2-(diphenylphosphino)pyridine) as the catalyst at 100 °C for 3 h. The coupling reaction can be carried out smoothly regardless of the electron-donating or electron-withdrawing group on the aromatic ring of organic thioaluminum reagents or aryl terminal alkynes. In addition, the broad substrate scope and the typical maintenance of vigorous efficiency on the gram scale make this protocol a potentially practical method to synthesize alkynyl sulfides. On the basis of the experimental results, a possible catalytic cycle has been proposed.

This paper demonstrates the synthesis, crystal structures, and amine recognition properties of a series of thiacopillar[5]arenes 1-4. A simple route for the thiolation of pillar[5]arene that allows for the easy synthesis of bis-pillar[5]arene structures is provided. Hence, synthesis of disulfide-linked bis-pillar[5]arenes 2 and 2a is reported, for the first time, from our newly developed copillar[5]arene precursor 1. Michael addition of the thiols to the quinone motif yields thiacopillar[5]arenes 3 and 4 from pillar quinone. In the study, the chemical properties of the thiocarbonate ring and phenolic ─OH in 1 are undertaken to demonstrate amine recognition. It visually detects 1,3-diaminopropane and 1,4-diaminobutane (putrescine) in DMSO through host-guest interaction, phenol deprotonation, and cleavage of the cyclic thiocarbonate ring. In reference to this, bis-pillararene 2 exhibits color change with different amines (except aromatic amines) and anions, giving no selectivity. Due to the absence of a hydroquinone motif in the structure, 2a does not exhibit similar characteristics. Furthermore, bis-pillararene 2 is established to be excellent in the vapor phase detection of volatile amines. On the other hand, 3 and 4 are insensitive in amine recognition due to the lack of disulfide bonds. A DFT study has been used to interpret the results.

Methanol synthesis typically occurs using syngas (CO, CO2, and H2) over Cu/ZnO/Al2O3 catalyst. However, this process involves a lot of ambiguities related to the nature of active site, the relative role of CO and CO2, the importance of metal-support interaction and the true source of C in methanol. Motivated by these challenges, it is computationally studied UiO-68 supported N-heterocyclic carbene-based coinage metal hydrides (NHC-M(I)-H) as single-atom catalysts for methanol synthesis, focusing specifically on CO hydrogenation as a simplified and efficient route. The study confirms that NHC-Cu(I)-H can catalyze methanol synthesis with CO as the only C source. Hence, it can eliminate CO2 from the reaction mixture which will otherwise complicate product separation due to water formation. Moreover, methanol synthesis from CO is more hydrogen-efficient and energy saving compared to that from CO2. The calculated activation barrier of methanol synthesis from CO over UiO-68 supported NHC-Cu(I)-H catalyst is lower than those reported for methanol synthesis from CO2 over various Cu-surfaces and nobel metal-based catalysts. Overall, the study demonstrates that CO hydrogenation over UiO-68 supported NHC-Cu(I)-H is not only a viable and efficient route for methanol production but also provides an attractive alternative to traditional Cu/ZnO/Al2O3-based systems.

Identification of proper inorganic coagulant for treatment of industrial wastewater contaminated with printing inks through coagulation-flocculation in absence and presence of polyacrylamide: Nanoparticle emissions and mechanical stability.

A rhodamine B-based fluorescent probe for Hg2+ and its analytical applications.

Construction of an effective colorimetric and fluorescent dual-mode microneedle patch for non-destructive detection of nitrite in pickling foods.

A simple and efficient synthetic route to the I2-promoted tandem annulation of N-(2-vinyl)phenylindoles and diaryl diselenides has been developed for the preparation of seleno-indolo[1,2-a]indole derivatives. Research has shown that iodine is an important reagent for triggering reactions and plays a crucial role in the reaction process. This reaction represents the first example of selenation reaction of 3-methyl-N-(2-vinylphenyl)-1H-indoles and diaryl diselenides under air conditions. Moreover, the reaction features a wide substrate scope, good group tolerance, and a low-cost iodine reagent, which provides a valuable strategy for the synthesis of polycyclic indole skeletons.

An atomically dispersed rhodium on TiO2 catalyst enables a tandem process, combining hydrogenative reduction with α,β-hydrogen–deuterium exchange of cinnamic acid, in which D2O serves as the deuterium source. In contrast with previous reductive deuteration methods that yield only partially labeled 3-phenylpropanoic acids (Dα-inc.: ≤50%, Dβ-inc.: ≤50%), this heterogeneous system delivers near-quantitative deuterium incorporation (Dα-inc.: 94%, Dβ-inc.: 99%) under mild conditions, outperforming Rh nanoparticles and homogeneous Rh catalysts. Mechanistic studies indicate that α-C–H activation is the slowest transformation step within the overall process, owing to the exceptional C–H bond activation capability of the atomically dispersed catalyst; efficient α-C–H hydrogen–deuterium exchange is readily achieved. In addition, although catalyst recyclability is constrained by Rh aggregation, no Rh leaching is detected. This work provides a concise, operationally simple route to alkyl fully deuterated 3-phenylpropanoic acids (d4-PA) and showcases the application of an atomically dispersed catalyst in tackling challenging deuterium-labeling transformations.

A nanospherical composite based on poly(2-chlorobenzenamine) and silver chloride (POCBA/AgCl NS-composite) was synthesized through a facile one-step, one-pot approach, providing a simple and efficient route to integrate conducting polymers with silver halides for advanced energy storage applications. The composite was thoroughly characterized, with XRD confirming its high crystallinity and semiconducting nature, while XPS validated the successful chemical integration and revealed the electronic environment of the constituent elements. Morphological analyses demonstrated the formation of uniform, porous nanospheres (∼180 nm), which facilitate rapid ion diffusion and effective electroactive surface utilization. Electrochemical evaluation in a pseudo-supercapacitor configuration revealed a high specific capacitance of 105 F g −1 at 0.1 A g −1 , retaining 86 F g −1 at 0.2 A g −1 , with an energy density of 8.8 Wh kg −1 . The device also exhibited low internal resistance (7.5 Ω) and outstanding cycling stability, maintaining 98.3% capacitance over 1000 charge–discharge cycles. Compared to previously reported polymer/silver halide composites, the single-step synthesized POCBA/AgCl NS-composite uniquely combines facile fabrication, high electrochemical performance, and excellent long-term durability, highlighting its potential as a next-generation pseudocapacitive material. This work demonstrates a novel strategy to engineer polymer–metal halide nanostructures, paving the way for efficient, reliable, and scalable energy storage devices.

Facile synthesis of high loading and highly electron-delocalized Co single-atom catalyst for PMS activation: An in-depth study of molecular orbital and catalytic mechanisms.

Silicon is an attractive platform for optoelectronic integration, but its indirect bandgap makes it a weak light emitter. Here, we demonstrate that sol-gel-derived silica (SiO2) coatings, when thermally annealed, can significantly boost silicon bandgap photoluminescence (PL). Samples annealed at 900 °C exhibit a more than fourfold increase in emission intensity near 1160 nm compared to as-deposited films. High-resolution Transmission Electron Microscopy (TEM), combined with geometric phase analysis (GPA), revealed that as-deposited samples exhibit relatively uniform interfacial strain of less than ±0.1%, whereas annealing at 900 °C introduces local strain fluctuations of up to ±2.0%. These nanoscale strain variations correlate directly with the observed PL enhancement. Detailed analysis using high-resolution TEM (HRTEM) and scanning transmission electron microscopy with electron energy-loss spectroscopy (STEM-EELS) reveals the reduction of annealing-induced defects in Si and the densification of the silica layer. These modifications alter the electronic states at the interface, as reflected in changes in the joint density of states, thereby enabling more efficient radiative recombination. Finite difference time domain (FDTD) simulations suggest that the enhanced PL signal near 1160 nm is partly attributable to annealing-induced morphological changes in silica. Together, these findings demonstrate that sol-gel-derived SiO2/Si stacks provide a simple and low-cost route to enhance silicon emission through strain engineering, offering strong potential for integration into CMOS-compatible photonic systems and the development of future on-chip light sources and optical interconnects.

Transition metal sulfide nanoparticles have emerged as awesome candidates to replace conventional noble metal catalysts for electrocatalytic water-splitting due to their unique structure and low cost. The creation of vacancies, an increase in active surface area and optimization of the electronic structure will enhance the electrocatalytic performance. In this study, with sulfur vacancy (SV) defect engineering, we have grown Mo-doped NiS ultrathin nanosheets built from self-assembled nanoparticles in situ on nickel foam (Mo-NiS/NF) using a simple one-pot hydrothermal approach. Nickel ions originating from NF underwent a sulfation reaction with L-cysteine, while the heteroatom Mo was introduced into the NiS lattice to form SV. Compared to pure NiS grown on NF (NiS/NF) and Mo-doped NiS powders (Mo-NiS/P), Mo-NiS/NF showed outstanding catalytic performance, achieving a current density of 10 mA cm-2 (1.0 M KOH) at a low potential of 1.56 V. Simultaneously, density functional theory calculations confirmed that the heteroatom Mo and SV substantially reduced the hydrolytic Gibbs free energy barrier of NiS. This strategy is expected to provide a simple route for the preparation of other metal sulfide nanoparticles for practical applications in water splitting.

Water electrolysis for hydrogen, though widely studied, presents exciting opportunities for improvement beyond conventional energy and cost-intensive catalysts. Natural ores, being abundant and readily available, hold immense promise as sustainable sources of alternative energy materials. Here, this method offers a simple and low-cost route, not only to make 2D materials but also to develop electrocatalysts from earth-abundant ores. Synthesis of 2D Bi2S3 is demonstrated via Liquid phase exfoliation (LPE) of the naturally abundant bismuthinite ore. Sustainability of such 2D Bi2S3 is explored for hydrogen evolution reaction (HER) from alkaline fresh and simulated seawater. The exfoliated Bi2S3 exhibits an overpotential of 693 and 678 mV at 10 mA cm- 2 in alkaline fresh and simulated seawater with a durability up to 40h. From Density Functional Theory (DFT) based First-principles calculations, sulfur sites are found to bind H-intermediates strongly in comparison with bismuth sites. Sustainability is further investigated by life cycle calculation. A lower carbon footprint of the 2D Bi2S3 catalyst is observed under both alkaline fresh (21.13 kg CO2eq kg-1 H2) and simulated seawater (15.56 kg CO2eq kg-1 H2). This work extends a sustainable strategy to utilize earth-abundant natural source for fabricating efficient and durable HER electrocatalysts for future fuel.

Heterostructured Ni-BTC@ZIF-67 microtubes prepared by a simple room-temperature aqueous route for high-performance supercapacitors

Copper-manganese bimetallic oxide with excellent laccase-like activity for colorimetric detection of formaldehyde via the specific aldimine condensation reaction.

Facile synthesis, multimode and tunable luminescence, and multifunctional applications of rare earth ions activated lead-free double perovskite crystals

Triggering zinc oxide nanostructure with gold and silver nanoparticles: A SERS-active hybrid Plasmonic construct.

Antiplatelet therapy through inhibition of P2Y12 and phosphodiesterase receptors by novel synthesis 1,3-dicyclohexylpyrimidine-2,4(1H,3H)-dione derivatives with computational evaluation.

We first optimized a simple and low-cost polyol-based synthesis route for the preparation of stable and monodisperse sub-10 nm copper nanoparticles. Building on this robust approach, we extended the method to tin and succeeded in producing tin nanoparticles that stabilized in an unconventional α-Sn phase, which is remarkable given the metastable character of this phase under ambient conditions. The resulting α-Sn nanoparticles exhibited excellent resistance to oxidation, together with long-term colloidal stability in air, enabling further processing for potential applications. In both cases, inexpensive commercial precursors and mild conditions (80 °C, aqueous or polyol solvents, ascorbic acid as the sole reducing agent, and no inert atmosphere or additional stabilizers) were employed. The nanoparticles were characterized using TEM, UV-visible spectroscopy, ATR-FTIR, ICP-OES, and XPS.

Mixed-mode chromatography is increasingly valued for retaining analytes with diverse polarity and charge by integrating hydrophilic interaction (HILIC), reversed-phase (RPLC), and ion-exchange mechanisms. However, designing stationary phases that are both easy to synthesize and chromatographically versatile remains challenging. This study presents DEA-Mix-SP, a novel silica-based stationary phase functionalized with diethanolamine via [2-(3,4-epoxycyclohexyl)ethyl]trimethoxysilane, offering a simple synthetic route for broad-spectrum separation. Three variants with different ligand densities were characterized by elemental analysis, FTIR, SEM, and BET. The columns showed excellent separation for various analytes: nine nucleobases/nucleosides were resolved within 13min, achieving up to 35,000 theoretical plates per meter, and eight benzoic acid derivatives were fully separated in 9min with efficiencies up to 50,000 N/m. Alkylbenzenes, PAHs, Sudan dyes, phenols, and anilines were also effectively separated. Retention mechanisms were studied using quantitative parameters such as logD, logS, and pKa, confirming significant anion-exchange effects. Performance was compared with ACE C18 (RPLC) and aminopropyl (HILIC) columns: DEA-Mix-SP showed superior separation performance in HILIC over the aminopropyl column and better separation of phenols, benzoic acids, and anilines than ACE C18, while achieving comparable results for fully non-polar analytes like alkylbenzenes, Sudan dyes, and PAHs. DEA-Mix-SP thus combines cost-effectiveness and high mixed-mode selectivity, providing reliable separation for analytes with wide polarity and charge ranges, making it a strong option for pharmaceutical, environmental, and food analyses.