Traditional Synthesis Methods Research Articles

Paired Electro‐Synthesis of Remote Amino Alcohols with/in H2O

Amino alcohols, particularly remote amino alcohols and peptide alcohols, are valuable due to their functional diversity in biologically active compounds. However, traditional synthesis methods face significant challenges, making electrochemistry an attractive alternative. We have developed a mild and biocompatible sequential paired electrolysis strategy, leveraging copper‐electrocatalysis to synthesize diverse remote amino alcohols, including unnatural peptide alcohols. Both experimental results and density functional theory (DFT) calculations demonstrate that water serves as both the hydroxyl source and the solvent, facilitating the generation of CuH with Cu(I) at the cathode, which in turn reduces the aldehyde intermediates formed during the reaction.

PairedElectro-Synthesis of Remote Amino Alcohols with/in H2O.

Amino alcohols, particularly remote amino alcohols and peptide alcohols, are valuable due to their functional diversity in biologically active compounds. However, traditional synthesis methods face significant challenges, making electrochemistry an attractive alternative. We have developed a mild and biocompatible sequential paired electrolysis strategy, leveraging copper-electrocatalysis to synthesize diverse remote amino alcohols, including unnatural peptide alcohols. Both experimental results and density functional theory (DFT) calculations demonstrate that water serves as both the hydroxyl source and the solvent, facilitating the generation of CuH with Cu(I) at the cathode, which in turn reduces the aldehyde intermediates formed during the reaction.

Precise synthesis of cyclopropyl methyl ketone via proton transfer of 5-chloro-2-pentanone driven by hydrogen bonds

The traditional synthesis methods of cyclopropyl methyl ketone (CPMK) have some disadvantages such as low yield, slow reaction rate and unclear catalytic mechanism. To solve these problems, a new strategy is developed to synthesize CPMK from 5-chloro-2-pentanone (CPE) using 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). Experiment results show that the yield of CPMK reached a maximum of 96.5% in DBU at 40°C for 30min. The mechanism study shows that the hydrogen bond between DBU and CPE is the key to drive the deprotonation and cyclization of CPE. The hydrogen bond is formed between the N atom on C=N of DBU and the α-H on the methylene group associated with the carbonyl group on CPE. The catalyst DBU is converted into [DBUH]+Cl−, which can be reclaimed and recycled completely. The density functional theory (DFT) calculation confirmed the existence of molecular hydrogen bonds and proved that the hydrogen bond driving force is the key to the reaction. The hydrogen bond driven mechanism provides a new idea for the basic research of cyclization reaction.

A review on the green metal nanotechnology in monogastric animal health: current trends and future prospects.

Green nanotechnology is the emerging field of research in recent decades with growing interest rapidly. This integrates green chemistry with green engineering to avoid using toxic chemicals in the synthesis of organic nanomaterials. Green nanotechnology would create a huge potential for the use of nanoparticles for more sustainable utilization in improving animal health. Nanoparticles can be synthesised by physical, chemical and biological processes. Traditional methods for physical and chemical synthesis of nanoparticles are toxic to humans, animals and environmental health, which limits their usefulness. Green synthesis of nanoparticles via biological processes and their application in animal health could maximize the benefits of nanotechnology in terms of enhancing food animal health and production as well as minimize the undesirable impacts on Planetary Health. Recent advances in nanotechnology have meant different nanomaterials, especially those from metal sources, are now available for use in nanomedicine. Metal nanoparticles are one of the most widely researched in green nanotechnology, and the number of articles on this subject in food animal production is growing nowadays. Therefore, research on metal nanoparticles using green technologies have utmost importance. In this review, we report the recent advancement of green synthesized metal nanoparticles in terms of their utilization in monogastric animal health, elucidate the research gap in this field and provide recommendations for future prospects.

Exploring sustainable synthesis paths: a comprehensive review of environmentally friendly methods for fabricating nanomaterials through green chemistry approaches.

This comprehensive review delves into the burgeoning field of nanotechnology, where the synthesis of nanoparticles (NPs) is strategically tailored to specific applications. Embracing the principles of green chemistry, nanotechnology increasingly utilizes environmentally friendly materials, such as plant extracts or microorganisms, as capping or reducing agents and solvents in the synthesis process. Notably, plant-based synthesis demonstrates enhanced stability and faster rates compared to microorganisms. The synthesized materials exhibit unique properties ranging from antimicrobial and catalytic effects to antioxidant activities and they are finding applications across diverse fields. Green synthesis processes, characterized by mild conditions in terms of temperature and reagents, stand in stark contrast to traditional chemical synthesis methods. This review focuses on the synthesis of various metal and metal oxide NPs, including Ag, Au, Zn, Fe, Mg, Ti, Sn, Cu, Cd, Ni, Co, and Ag NPs and their oxides, using plant extracts and microorganisms. We provide a comprehensive analysis of the advantages, disadvantages, and applications associated with each synthesis method. Additionally, we explore the future prospects of green synthesis and its limitations and challenges, offering insights into its evolving role in nanotechnology.

Reversible Grafting in Surface Organometallic Chemistry with a Late Transition‐Metal Amidinate Precursor

Supported catalysts are central to industrial catalytic processes. While traditional synthesis methods often yield poorly defined materials, thus complicating structural elucidation, Surface Organometallic Chemistry (SOMC) offers a solution, producing well‐defined structures. Recent advances in SOMC precursor development have shown that amidinate‐based precursors are a privileged class of precursors to generate supported metallic nanoparticles. In that context, this study investigates the grafting mechanism of a prototypical amidinate precursor, Ir(COD)(DIA) (1‐Ir), onto SiO2. Unique to amidinate complexes, grafting is shown to occur without ligand release, creating a reversible covalent bond. Using Ir‐TBOS as a molecular analogue, the structure of the grafted species and the reversibility of the reaction with O‐H groups are demonstrated using IR spectroscopy, single X‐Ray diffraction, variable‐temperature NMR spectroscopy, X‐Ray absorption spectroscopy (XAS), and supported by DFT calculations. Notably, we show that a partial degrafting is also possible at elevated temperatures under vacuum

Photogeneration of β-Borylsilyl Radical via Decarboxylation of N-Hydroxyphthalimide Esters.

Gem-borylsilylalkanes are versatile intermediates in organic synthesis, and the traditional synthesis methods have mainly focused on metal reagents, the insertion reactions of diazo compounds, and hydrosilylation/hydroborylation reactions of unsaturated bonds. Herein, a novel, efficient gem-borylsilylalkanes synthesis via a radical approach is reported. This method introduced a β-gem-borylsilyl NHPI ester as the precursor of the β-borylsilyl radical that, coupling with radical acceptors under photo conditions, and the corresponding gem-borylsilylalkanes bearing unsaturated bonds, facilitate subsequent transformations.

Optimization, imaging and LHE analysis of magnesium oxide nanoparticles synthesized with carambola extract as natural dye sensitizer

This work explores the enhancement of dye-sensitized solar cells (DSSCs) by using magnesium oxide nanoparticles (MgO NPs) that have been green-synthesized, with carambola extract acting as a natural dye sensitizer. Green synthesis minimizes the negative effects of traditional synthesis methods on the environment by providing a sustainable and ecologically friendly way to produce MgO NPs. To increase their effectiveness in DSSC applications, the synthesized nanoparticles underwent optimization. The morphology and size distribution of MgO NPs were characterized by scanning electron microscopy (SEM), which revealed spherical forms with a consistent size distribution. The crystalline nature of the MgO NPs was verified by X-ray diffraction (XRD), which revealed distinctive peaks that correspond to the bulk MgO crystal planes. A band gap of 3.5 eV, appropriate for UV region absorption, was found using UV–visible spectroscopy. FT-IR (Fourier-transform infrared) spectroscopy revealed information about their molecular compositions. Positive electronic characteristics, such as a negative total energy change (ΔE_T) and a high electrophilicity index (ω), which indicates effective charge transfer, were found through computational analysis. The light harvesting efficiency (LHE) value of 0.00459 signifies optimal light absorption capability by the dye molecule. The outcomes show that MgO NPs that have undergone green synthesis have the potential to be efficient and stable sensitizers for DSSCs. In addition to highlighting the significance of green synthesis techniques in nanomaterial research for renewable energy applications, this work advances the development of efficient and sustainable solar energy systems.

Molecular Characterization of Endophytic Fungal Strains for Green Synthesis of ZnO and Au Nanoparticles

Abstract Introduction/Objective Introduction: Traditional methods for nanoparticle synthesis often involve hazardous compounds, posing environmental risks and limiting their biomedical applications due to instability. The exploration of green synthesis approaches using natural products and eco-friendly solvents presents a challenging yet imperative pursuit in nanoparticle research. Methods/Case Report Methods: Endophytic fungi were isolated from healthy Eucalyptus sideroxylon plants collected from the Desert Research Center. Cultivation of fungi in malt extract broth was conducted at 28°C with agitation for 96 hours. Subsequently, fungal DNA was extracted, and ITS-rDNA regions were PCR-amplified for identification. Sequencing and phylogenetic analysis were performed to characterize the fungal isolates. Fungal filtrates were utilized for the biosynthesis of ZnO and Au nanoparticles (NPs) from ZnSO4 and HAuCl4 solutions, respectively. Results (if a Case Study enter NA) Results: Among the 13 fungal isolates, Fusarium chlamydosporum (FI-03) exhibited the most efficient synthesis of ZnO and Au NPs. Sequencing confirmed the identity of the fungal strain. The synthesized NPs displayed uniform spherical shapes, with ZnO NPs averaging 19.3 nm and Au NPs averaging 22.1 nm in size. Transmission electron microscopy (TEM) analysis further elucidated the morphology of the NPs. Conclusion Conclusion: Fusarium chlamydosporum emerged as a promising candidate for the green synthesis of ZnO and Au NPs. This environmentally friendly approach offers a cost-effective and biocompatible alternative to conventional nanoparticle synthesis methods.

Biosynthesis of novel non-proteinogenic amino acids β-hydroxyenduracididine and β-methylphenylalanine in Escherichia coli.

Non-proteinogenic amino acids (npAAs) are valuable building blocks for the development of advanced pharmaceuticals and agrochemicals. The surge in interest in their synthesis is primarily due to the potential to enhance and diversify existing bioactive molecules. This can be achieved by altering these bioactive molecules to improve their effectiveness, reducing resistance compared to their natural counterparts or generating molecules with novel functions. Traditional production of npAAs in native hosts requires specialized conditions and complex cultivation media. Furthermore, these compounds are often found in organisms that challenge genetic manipulation. Thus, the recombinant production of these npAAs in a model organism like Escherichia coli paves the way for groundbreaking advancements in synthetic biology. Two synthetic operons, comprising of five heterologous proteins were genomically integrated into E. coli for the synthesis of npAAs β-methylphenylalanine (BmePhe), β-hydroxyenduracididine (BhEnd), and enduracididine (End). Proteomic and metabolomic analysis confirmed production of these compounds in E. coli for the first time. Interestingly, we discovered that the exogenous addition of pathway precursors to the E. coli system enhanced the yield of BmePhe by 2.5 times, whereas it concurrently attenuated the production of BhEnd and End, signifying a selective precursor-dependent yield enhancement. The synthetic biology landscape is broadened in this study by expanding the repertoire of amino acids beyond the conventional set of 22 standard proteinogenic amino acids. The biosynthesized npAAs, End, BhEnd, and BmePhe hold promise for engineering proteins with modified functions, integrating into novel metabolites and/or enhancing biological stability and activity. Additionally, these amino acids' biological production and subsequent purification present an alternative to traditional chemical synthesis methods, paving a direct pathway for pharmacological evaluation.

Production of Magnesium Dilactate through Lactic Acid Fermentation with Magnesium Carbonate.

Magnesium dilactate is increasingly sought after for its applications in the pharmaceutical, food, and dietary supplement industries due to its essential role in various physiological processes. This study explores a sustainable method for synthesizing magnesium dilactate through lactic acid fermentation using tomato juice, coupling the neutralization of lactic acid with hydrated magnesium carbonate hydroxide. Utilizing the lactic acid bacteria Lactobacillus paracasei and Lactobacillus plantarum, fermentation was optimized in a 50% diluted MRS medium supplemented with glucose and tomato juice supplemented with glucose, yielding a maximum lactate concentration of 107 g/L. Notably, fermentation in diluted media proved more effective than in undiluted tomato juice, highlighting the inhibitory effects of certain organic compounds and the physical nature of the original tomato juice. Post-fermentation, magnesium lactate was crystallized, achieving high recovery rates of up to 95.9%. Characterization of the product through X-ray diffraction and scanning electron microscopy confirmed its crystalline purity. This research underscores the viability of tomato juice as a fermentation substrate, promoting the valorization of agricultural by-products while providing an eco-friendly alternative to traditional chemical synthesis methods for magnesium dilactate production.

Microwave-assisted Synthesis of Benzimidazole Derivatives: A Green and Effective Approach

Benzimidazole derivatives are pivotal in medicinal chemistry due to their diverse therapeutic applications. Traditional synthesis methods often require catalysts and long reaction times, which can be inefficient and environmentally unfriendly. Hence, there is a growing need for more efficient and eco-friendly synthetic methodologies. A newly devised and efficacious synthetic methodology has been established for the synthesis of benzimidazole derivatives, employing microwave assistance without the requirement for a catalyst. This method facilitated the synthesis of fifteen derivatives with notable efficiency, characterized by significantly reduced reaction times ranging from 5 to 10 minutes and impressive yields ranging from 94% to 98%. The identity and purity of the synthesized benzimidazole derivatives were meticulously verified through a comprehensive analysis, encompassing a comparison of their physicochemical properties and spectral characteristics with authenticated reference data. This method represents a significant advancement in the synthesis of benzimidazole derivatives, offering a rapid and high-yielding alternative to traditional synthetic routes.

Ixora Coccinea Extract for Biosynthesis of Titanium Dioxide Nanoparticles: A Precursor for Organic Electronics

This study explores the synthesis, characterization, and evaluation of titanium dioxide nanoparticles (TiO2NPs) as a precursor for the electron transport layer in organic electronics. Traditional physical and chemical synthesis methods are not environmentally friendly or economical, due to the use of toxic chemicals and high energy. However, biosynthesis offers a low-cost, eco-friendly alternative. The synthesized NPs were characterized using various techniques, including X-ray diffraction technique, transmission electron microscopy, scanning electron microscopy, Fourier Transform Infra-red microscopy, electron dispersive X-ray, and UV-visible spectroscopy with a four-point probe equipped with Keithley2400 source meter. Results showed high crystallinity and a band gap energy of 4.02 eV. Electrical properties show sheet resistance, resistivity and conductivity as 67.22 x 106 Ω, 1.71 x 106 Ωm-1 and 0.585 x-6 Sm-1 respectively which were promising, with better photovoltaic characteristics than pure titanium dioxide. These properties suggest potential applications as an electron transport layer for solar cell technology.

Free-standing cubic gauche nitrogen stable at 760 K under ambient pressure.

Cubic gauche nitrogen (cg-N) has received wide attention for its exceptionally high energy density and environmental friendliness. However, traditional synthesis methods for cg-N predominantly rely on high-pressure techniques or the utilization of nanoconfined effects using highly toxic and sensitive sodium azide as precursor, which substantially restrict its practical application. On the basis of the first-principles simulations, we found that adsorption of potassium on the cg-N surface exhibits superior stabilization compared to sodium. Then, we chose safer potassium azide as precursor for synthesizing cg-N. Through plasma-enhanced chemical vapor deposition treatment, the free-standing cg-N was successfully synthesized without the need for high-pressure and nanoconfined effects. It demonstrated excellent thermal stability up to 760 K, and then rapid and intense thermal decomposition occurred, exhibiting typical thermal decomposition behaviors of high-energy-density materials. The explosion parameters were also measured using laser-induced plasma spectroscopy. Our work has substantially promoted the practical application of cg-N as HEDMs.

Prussian White/Reduced Graphene Oxide Composite as Cathode Material to Enhance the Electrochemical Performance of Sodium-Ion Battery.

Prussian white (PW) is considered a promising cathode material for sodium-ion batteries. However, challenges, such as lattice defects and poor conductivity limit its application. Herein, the composite materials of manganese-iron based Prussian white and reduced graphene oxide (PW/rGO) were synthesized via a one-step in situ synthesis method with sodium citrate, which was employed both as a chelating agent to control the reaction rate during the coprecipitation process of PW synthesis and as a reducing agent for GO. The low precipitation speed helps minimize lattice defects, while rGO enhances electrical conductivity. Furthermore, the one-step in situ synthesis method is simpler and more efficient than the traditional synthesis method. Compared with pure PW, the PW/rGO composites exhibit significantly improved electrochemical properties. Cycling performance tests indicated that the PW/rGO-10 sample exhibited the highest initial discharge capacity and the best cyclic stability. The PW/rGO-10 has an initial discharge capacity of 128 mAh g-1 at 0.1 C (1 C = 170 mA g-1), and retains 49.53% capacity retention after 100 cycles, while the PW only delivers 112 mAh g-1 with a capacity retention of 17.79% after 100 cycles. Moreover, PW/rGO-10 also shows better rate performance and higher sodium ion diffusion coefficient (DNa+) than the PW sample. Therefore, the incorporation of rGO not only enhances the electrical conductivity but also promotes the rapid diffusion of sodium ions, effectively improving the electrochemical performance of the composite as a cathode material for sodium-ion batteries.

Palladium nanoparticles incorporated biogenic modified graphitic carbon nitride as an electrocatalyst for methanol oxidation reaction

This research explores palladium (Pd) nanoparticles supported on graphitic carbonitride (g-C3N4) as a cost-effective and CO tolerant catalyst towards electrocatalytic methanol oxidation reaction (MOR). The study delves into the green synthesis strategy, employing phytochemicals as reducing, capping and stabilizing agents. This approach aligns with environmentally friendly practices, steering away from hazardous chemicals and solvents commonly used in traditional synthesis methods. The synthesis involves the dispersion of Pd nanoparticles supported on graphitic carbon nitride (g-C3N4) modified by banana leaf extract [PdNPs@g-C3N4-BLE]. The obtained nanocatalyst is characterized using various spectroscopic and microscopic techniques. Further, the synthesized PdNPs@g-C3N4-BLE is utilized as electrocatalyst for methanol oxidation reaction (MOR) in basic medium (1 M KOH). PdNPs@g-C3N4-BLE shows satisfactory activity towards MOR with an onset potential of 0.834 V and current density of 6.795 mA/cm2 at 1.0 V.

High-efficiency RbASiF6:Mn4+ (A = K, Cs) phosphors obtained by one-step green synthesis method

Red-emitting Mn4+-doped fluoride phosphors are recognized as promising materials for high-performance warm white light-emitting diodes (WLEDs). However, the extensive use of toxic hydrofluoric acid in traditional synthesis methods hinders their development and commercialization. Furthermore, the traditional solid-phase method often has cumbersome sintering steps, high temperature, long holding time, and certain safety hazards, so it is very necessary to develop a green synthesis method with simple steps and low energy consumption. In this study, a low-temperature solid-state method is proposed to synthesize RbASiF6:Mn4+ (A = K, Cs) phosphors by one step. Optimal emission intensities were observed at Mn4+ concentrations of 1.2 % in RbKSiF6 and 2.1 % in RbCsSiF6. These phosphors demonstrated high thermal stability. At 423 K, the photoluminescence intensities of RbKSiF6:1.2 %Mn4+ and RbCsSiF6:2.1 %Mn4+ reached 114 % and 87 % of their respective values at room temperature. Meanwhile, the chromaticity shifts were almost negligible, and high color purity was achieved for both phosphors. The electro-optical performance of WLED devices utilizing these phosphors, in combination with YAG:Ce3+ and GaN chips, showed high color rendering indices (CRI) and low correlated color temperatures (CCT) across varying currents. Specifically, under a driving current of 20 mA, the device incorporating RbKSiF6:1.2 %Mn4+ exhibited a CRI of 94 and a CCT of 3732 K, with a luminous efficacy of 61 lm/W. These findings highlight the potential of green-synthesized RASFM phosphors in advancing the application of warm WLEDs.

Heterogenous Copper(0)-Assisted Dopamine Oxidation: A New Pathway to Controllable and Scalable Polydopamine Synthesis.

In this study, we introduce an approach for synthesizing polydopamine (PDA) through the controlled oxidation of dopamine using metallic copper. Traditional methods of PDA synthesis often encounter challenges such as scalability, reproducibility, and control over polymerization. Our approach utilizes the catalytic properties of metallic copper in the presence of dissolved oxygen to generate reactive oxygen species (ROS) without additional chemicals. This process allows for precise control over dopamine oxidation, leading to reliable, materials and cost-effective upscalable PDA production. We investigated the reaction kinetics and the role of copper and ROS in dopamine oxidation, using several different experimental techniques. Our results demonstrate that, even at low pH, the copper-assisted method produces PDA with properties comparable to those synthesized through conventional means. We propose a mechanism for PDA synthesis that is initiated by oxygen adsorption onto copper surface, leading to the generation of various ROS which act as oxidizing agents in PDA synthesis. This method presents an advancement in the scalable and controlled production of PDA, with potential applications in various scientific and industrial fields.

Impact of metal precursor and molar ratios on adsorption and separation of CO2 and CH4 by SOD-ZIF-67 prepared using green solvent-free synthesis

The subclass of metal-organic frameworks (MOFs) known as SOD-ZIF-67 (Sodalite Co (mIm)2, with mIm = 2-methylimidazole) has demonstrated exceptional performance in carbon dioxide (CO2) adsorption and separation. Traditional synthesis methods for SOD-ZIF-67 are often time-consuming and require significant quantities of organic solvents. This study introduces an enhanced, eco-friendly, solvent-free method for synthesizing SOD-ZIF-67. In this approach, SOD-ZIF-67 is produced within 1 h by mechanically grinding a cobalt (Co) metal precursor with an organic linker (mIm), eliminating the need for solvents. The properties of the synthesized SOD-ZIF-67 samples were confirmed through various characterization techniques. Thermal stability tests indicated that the synthesized SOD-ZIF-67 could endure temperatures up to 673 K. Among the samples prepared with different molar ratios, the SOD-ZIF-67 sample with a Co to HmIm molar ratio of 2:1 (denoted as Z-2) demonstrated the highest BET surface area and pore volume, measuring 1923 m2/g and 0.72 cm3/g, respectively. Z-2 exhibited uniform and narrow ultramicropores measuring 0.54 nm, and demonstrated a CO2 adsorption capacity of 91.52 mg (CO2)/g (2.08 mmol/g) at 298 K and 100 kPa. The material showed high selectivity for CO2 over N2 and CH4, with selectivities of 20.44 for CO2/N2 (0.15:0.85) and 4.28 for CO2/CH4 (0.5:0.5). Additionally, breakthrough experiments with CO2/N2 and CO2/CH4 mixtures validated its dynamic separation efficiency, underscoring Z-2′s suitability for selective CO2 capture from flue gases and natural gas purification.

A bioinspired Fe/Mo bimetallic nitride catalyst for efficient electrochemical ammonia synthesis and Zn-nitrate battery

The electrocatalytic nitrate reduction reaction to ammonia (NRA) offers a promising alternative to traditional ammonia synthesis methods. In nature, enzymes containing molybdenum and iron sites catalyze the reduction of nitrate and nitrite ions. Drawing inspiration from these enzymes, we synthesized a carbon-coated nano-octahedra of FeMo-based nitride (FeMoN@C NO) by pyrolyzing phosphomolybdic acid hydrate (POM) doped Fe-NH2-MIL-101 to catalyze NRA. Experimental results demonstrate that in an alkaline environment, FeMoN@C NO exhibits a suitable hydrogen evolution reaction (HER) capacity, and the protons or hydroxyls produced effectively facilitate the hydrogenation reaction in the ammonia synthesis process. Additionally, the introduction of Mo increases the number of active sites and effectively reduces the thermodynamic barrier in NRA, thereby enhancing the rate of ammonia synthesis. As a result, FeMoN@C NO displays outstanding NH3 Faradaic efficiency (FE) of 98.2 % and an NH3 yield of 434.16 µmol/h cm−2. Building upon the excellent electrocatalytic properties of FeMoN@C NO, a new Zn-nitrate battery system is assembled in this work, which exhibits an outstanding peak power density of 3.23 mW cm−2 and an FE of 91.58 % for NH3 production. This work provides a new perspective for designing enzyme-mimicking nitrate reduction catalysts and broadens the application of Zn-based batteries.