Microwave-assisted Synthesis of Al_(4)SiC_(4) and Its Effect on Properties of MgO-C Refractories

Al_(4)SiC_(4) was synthesized from Al powder, silicon carbide, and graphite by microwave sintering, and characterized by XRD and SEM. Then the synthesized material was added to the magnesia carbon refractory brick to study its effect on the oxidation resistance, apparent porosity, bulk density, elastic modulus, and modulus of rupture. It is found that Al_(4)SiC_(4) can be synthesized by microwave sintering at 1 300 ℃ and the addition of Al_(4)SiC_(4)-containing material as an antioxidant can enhance the oxidation resistance of the magnesia carbon refractory brick.

Green Chemistry Allometry Test of Microwave-Assisted Synthesis of Transition Metal Nanostructures

Microwave irradiation is considered an important approach to Green Chemistry, because of its ability to rapidly increase the internal temperature of polar-organic compounds that lead to synthesis times of minutes rather than hours when compared to conventional thermal heating. This works describes a dual allometry test for the discrimination between the solvents and reagents used in the microwave-assisted synthesis of transition metal (zinc oxide, palladium silver, platinum, and gold) nanostructures. The test is performed in log-log process energy phase-space projection, where the synthesis data (kJ against kJ·mol-1) has a power-law signature. The test is shown to discriminate between recommended Green Chemistry, problematic Green Chemistry, and Green Chemistry hazardous solvents. Typically, recommended Green chemistry exhibits a broad y-axes distribution within an upper exponent = 1 and lower exponent = 0.5. Problematic Green Chemistry exhibits a y-axes narrower distribution with an upper exponent = 0.94 and lower exponent = 0.64. Non-Green Chemistry hazardous data exhibits a further narrowing of the y-axes distribution within upper exponent = 0.87 and lower exponent = 0.66. In all three cases, the y-axes is aligned to original database power-law signature. It is also shown that in the x-axes direction (process energy budget) the grouped order of magnitude decreases from four orders for recommended Green Chemistry solvent and reagent data, through two orders for non-Green Chemistry hazardous material and down to one order for problematic Green Chemistry.

Microwave-assisted synthesis of asymmetric thiocarbonohydrazones under solvent-free conditions

Six new asymmetric thiocarbonohydrazones 3a-3f were synthesized from following steps： firstly hydrazine hydrate reacted with carbon disulfide to form thiocarbonohydrazide （1） under microwave irradiation. Then compound （1） reacted with ketone and different aldehydes step by step to give 3a-3f with excellent yields under solvent-free conditions using microwave irradiation. Their structures have been determined by elemental analysis, IR, MS and ^1H NMR data. 2009 Qing Han Li. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

Fast, green microwave-assisted synthesis of single crystalline Sb_2Se_3 nanowires towards promising lithium storage

In this work, a fast(0.5 h), green microwave-assisted synthesis of single crystalline Sb_2Se_3 nanowires was developed. For the first time we demonstrated a facile solvent-mediated process, whereby intriguing nanostructures including antimony selenide(Sb_2Se_3) nanowires and selenium(Se) microrods can be achieved by merely varying the volume ratio of ethylene glycol(EG) and H_2O free from expensive chemical and additional surfactant. The achieved uniform Sb_2Se_3 nanowire is single crystalline along [001]growth direction with a diameter of 100 nm and a length up to tens of micrometers. When evaluated as an anode of lithium-ion battery, Sb_2Se_3 nanowire can deliver a high reversible capacity of 650.2 m Ah g^(-1) at 100 mA g^(-1) and a capacity retention of 63.8% after long-term 1000 cycles at 1000 mA g^(-1), as well as superior rate capability(389.5 m Ah g^(-1) at 2000 mA g^(-1)). This easy solvent-mediated microwave synthesis approach exhibits its great universe and importance towards the fabrication of high-performance metal chalcogenide electrode materials for future low-cost, large-scale energy storage systems.

A convenient microwave-assisted synthesis of cinchona alkaloid-derived ligands

An efficient synthesis of cinchona alkaloid-derived ligands based on solvent-free microwave-assisted reaction was described. The coupling of 1,4-dichlorophthalazine or 3,6-dichloropyridazine with quinine, cinchonine or cinchonidine provide bis-or monocinchona alkaloid-derived ligands in moderate to good yields （52-89%） within 15 min under optimum microwave conditions.

Microwave-assisted synthesis and characterization of ZnO-nanorod arrays

High density ZnO-nanorod arrays(rod length 1.59μm)were successfully synthesized via a microwave-assisted solution-phase method using zinc chloride and ammonia solution as reactants.The influence of concentration of ammonia solution, work power,and microwave irradiation time on the morphology and size of final products was carefully investigated.The crystal structure,chemical composition and morphologies of final products were characterized using X-ray powder diffraction(XRD), scanning electron microscopy(SEM)and photoluminescence(PL).The as-synthesized ZnO is composed of single crystalline and possesses three photoluminescence emissions centered at 400,469 and 534.5 nm,respectively.

Mass-Based Environmental Factor and Energy Assessment of Microwave-Assisted Synthesized Transition Metal Nanostructures

This paper describes mass-based energy phase-space projection of microwave-assisted synthesis of transition metals (zinc oxide, palladium, silver, platinum, and gold) nanostructures. The projection uses process energy budget (measured in kJ) on the horizontal axes and process density (measured in kJg−1) on the vertical axes. These two axes allow both mass usage efficiency (Environmental-Factor) and energy efficiency to be evaluated for a range of microwave applicator and metal synthesis. The metrics are allied to the: second, sixth and eleventh principle of the twelve principle of Green Chemistry. This analytical approach to microwave synthesis (widely considered as a useful Green Chemistry energy source) allows a quantified dynamic environmental quotient to be given to renewable plant-based biomass associated with the reduction of the metal precursors. Thus allowing a degree of quantification of claimed “eco-friendly” and “sustainable” synthesis with regard to waste production and energy usage.

Optimization of microwave-assisted synthesis of N^1-ethoxymethyl-substituted cyclic inosine diphosphoribose and its analogues

An optimized approach for the synthesis of N^1-ethoxymethyl-substituted cyclic inosine diphosphoribose（cIDPRE）,an analogue of cyclic adenosine diphosphoribose（cADPR）,has been developed via microwave-assisted intramolecular cyclization. The target compound has been successfully obtained through N^1-substitution,phosphorylation,cyclization and deprotection.By using this method,8-amino and bromo-substituted cIDPRE analogues were successfully obtained in good yield.The new approach has greatly shortened the synthetic route and enhanced the overall efficiency.

Microwave-assisted synthesis of some novel fluorinated pyrazolo[3,4-d]pyrimidine derivatives containing 1,3,4-thiadiazole as potential antitumor agents

A facile microwave-assisted procedure for synthesis of novel fluorinated pyrazolo[3,4-d]pyrimidine derivatives containing 1,3,4-thiadiazole is described. This protocol presented such advantages as short reaction time, high yields, simple purification and environmentally benign procedures. Their antitumor activities were evaluated against HL-60 by an MTT assay. The preliminary results indicated that some title compounds exhibit more potent antitumor inhibitory activity than doxorubicin （DOX）.

Microwave-assisted synthesis of nanoscale Eu(BTC)(H_2O)·DMF with tunable luminescence

Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray powder diffraction （XRD）, thermal gravimetric analysis （TGA） and Fourier-transform infrared spectra （FTIR） analyses. Eu（BTC）（H20）.DMF with various morphologies, including particle-like, rod-like, straw-sheaf-like nanostructures, could be simply prepared by con- trolling the concentrations of the starting reactants. The optical measurements on the obtained Eu（BTC）（H20）- DMF indicated that all the nanomaterials show the characteristic emissions of the Eu3＋ ions at 578, 590, 612, 650, and 699 nm, which were at- tributed to 5Do→7FJ （J=0-4） transitions of the Eu3＋ ion, respectively. It was also noticed that the luminescent properties of the as-prepared products were heavily dependent on the morphologies and sizes of the nanomaterials. The assembled straw-sheaf-like architectures displayed the strongest emissions and the longest luminescence lifetime, which was mainly due to the fewest surface defects.

Facile Microwave-Assisted Synthesis of 2D Imine-Linked Covalent Organic Frameworks for Exceptional Iodine Capture

Covalent organic frameworks(COFs)have emerged as auspicious porous adsorbents for radioiodine capture.However,their conventional solvothermal synthesis demands multiday synthetic times and anaerobic conditions,largely hampering their practical use.To tackle these challenges,we present a facile microwave-assisted synthesis of 2D imine-linked COFs,Mw-TFB-BD-X,(X=−CH_(3) and−OCH_(3))under air within just 1 h.The resultant COFs possessed higher crystallinity,better yields,and more uniform morphology than their solvothermal counterparts.Remarkably,Mw-TFB-BD-CH_(3) and Mw-TFB-BDOCH_(3) exhibited exceptional iodine adsorption capacities of 7.83 g g^(−1) and 7.05 g g^(−1),respectively,placing them among the bestperforming COF adsorbents for static iodine vapor capture.Moreover,Mw-TFB-BD-CH_(3) and Mw-TFB-BD-OCH_(3) can be reused 5 times with no apparent loss in the adsorption capacity.The exceptionally high iodine adsorption capacities and excellent reusability of COFs were mainly attributed to their uniform spherical morphology and enhanced chemical stability due to the in-built electron-donating groups,despite their low surface areas.This work establishes a benchmark for developing advanced iodine adsorbents that combine fast kinetics,high capacity,excellent reusability,and facile rapid synthesis,a set of appealing features that remain challenging to merge in COF adsorbents so far.

Microwave-assisted synthesis of 3D flowerlike a-Ni(OH)_2 nanostructures for supercapacitor application

Three-dimensional flowerlike α-Ni（OH）2 nanostructures were successfully synthesized by the microwave-assisted reflux as short as 30 rain. The crystalline structure and morphology of the products were characterized by X-ray diffraction, N2 adsorption-desorption isotherms, field emission scanning electron microscopy, and transmission electron microscopy. The α-Ni（OH）2 nanostructure shows a large surface area of 173 m2 g-1 and narrow mesopore distribution. The electrochemical properties of the as-prepared α-Ni（OH）2 as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 6 mol/L KOH electrolyte. The α-Ni（OH）2 nanostructure shows a maximum specific capacitance of 2030 F g-1 at a current density of 1 A g-1 and exhibits excellent rate capability. These results suggest that it is a promising electrode material for supercapacitor application.

Microwave-assisted synthesis and antimicrobial activities of 2-aryl-3-(naphthalene-1 or 2-yl)-1,3-thiazolidin-4-ones

2-aryl-3-(naphthalene-1 or 2-yl)-1,3-thiazolidin-4-ones 4 and 5 were synthesized in 41%–67%yield by using microwave-assisted one-pot protocol.The structures of the new compounds 4l,4m,5c,5e,5g,5h,and 5j–5m were confirmed by IR,NMR,MS,and elemental analysis.The antimicrobial activities of the compounds against Pseudomonas syringae pv.lachrymans(Smith et Bryan)Young,Dye&Wilkie,Botrytis cinerea Pers.,and Sphaerotheca fusca Blum.were examined.Some of the compounds showed good antifungical activity against Sphaerotheca fusca Blum.

Microwave-Assisted Transition Metal Nanostructure Synthesis: Power-Law Signature Verification

A power-law (y = cxn) signature between process energy budget (kJ) and process energy density (kJ·ml-1) of microwave-assisted synthesis of silver and gold nanostructures has been recently described [Law and Denis. AJAC, 14(4), 149-174, (2023)]. This study explores this relation further for palladium, platinum, and zinc oxide nanostructures. Parametric cluster analysis and statistical analysis is used to test the power-law signature of over four orders of magnitude as a function of six microwave applicator-types metal precursor, non-Green Chemistry synthesis and claimed Green Chemistry. It is found that for the claimed Green Chemistry, process energy budget ranges from 0.291 to 900 kJ, with a residual error ranging between −33 to +25.9 kJ·ml-1. The non-Green Chemistry synthesis has a higher process energy budget range from 3.2 kJ to 3.3 MJ, with a residual error of −33.3 to +245.3 kJ·ml-1. It is also found that the energy profile over time produced by software controlled digestion applicators is poorly reported which leads to residual error problematic outliers that produce possible phase-transition in the power-law signature. The original Au and Ag database and new Pd, Pt and ZnO database (with and without problematic outliers) yield a global microwave-assisted synthesis power-law signature constants of c = 0.7172 ± 0.3214 kJ·ml-1 at x-axes = 0.001 kJ, and the exponent, n = 0.791 ± 0.055. The information in this study is aimed to understand variations in historical microwave-assisted synthesis processes, and develop new scale-out synthesis through process intensification.

Microwave-Assisted Au and Ag Nanoparticle Synthesis: An Energy Phase-Space Projection Analysis

Microwave-assisted synthesis of gold and silver nanoparticles, as a function of Green Chemistry, non Green Chemistry, and four applicator types are reported. The applicator types are Domestic microwave ovens, commercial temperature controlled microwave chemistry ovens (TCMC), digesters, and axial field helical antennae. For each of these microwave applicators the process energy budget where estimated (Watts multiplied by process time = kJ) and energy density (applied energy divided by suspension volume = kJ·ml-1) range between 180 ± 176.8 kJ, and 79.5 ± 79 kJ·ml-1, respectively. The axial field helical field an-tenna applicator is found to be the most energy efficient (0.253 kJ·m-1 per kJ, at 36 W). Followed by microwave ovens (4.47 ± 3.9 kJ·ml-1 per 76.83 ± 39 kJ), and TCMC ovens (2.86 ± 2.3 kJ·m-1 per 343 ± 321.5 kJ). The digester applicators have the least energy efficiency (36.2 ± 50.7 kJ·m-1 per 1010 ± 620 kJ). A comparison with reconstructed ‘non-thermal’ microwave oven inactivation microorganism experiments yields a power-law signature of n = 0.846 (R2 = 0.7923) four orders of magnitude. The paper provides a discussion on the Au and Ag nanoparticle chemistry and bio-chemistry synthesis aspects of the microwave applicator energy datasets and variation within each dataset. The visual and analytical approach within the energy phase-space projection enables a nanoparticle synthesis route to be systematically characterized, and where changes to the synthesis are to be mapped and compared directly with historical datasets. In order to help identify lower cost nanoparticle synthesis, in addition to potentially reduce synthesis energy to routes informed changes to potentially reduce synthesis energy budget, along with nanoparticle morphology and yield.

Navigating the pathways:TAR-DNA-binding-protein-43 aggregation,axonal transport,and local synthesis in amyotrophic lateral sclerosis pathology

Neurons are highly polarized cells with axons reaching over a meter long in adult humans.To survive and maintain their proper function,neurons depend on specific mechanisms that regulate spatiotemporal signaling and metabolic events,which need to be carried out at the right place,time,and intensity.Such mechanisms include axonal transport,local synthesis,and liquid-liquid phase separations.Alterations and malfunctions in these processes are correlated to neurodegenerative diseases such as amyotrophic lateral sclerosis(ALS).

Triazatruxene-containing hyperbranched polymers:Microwave-assisted synthesis and optoelectronic properties

Hyperbranched polymer structures represent a class of high-functionality building blocks with excellent three-dimensional topology for the construction of highly substituted conjugated polymers.In this contribution,an efficient microwave synthesis protocol toward the synthesis of conjugated hyperbranched polymers is presented.A novel series of soluble hyperbranched polyfluorenes (PTF1-PTF3) incorporating triazatruxene moiety as the branch units with various branching degrees have thus been successfully constructed with good yields and high molecular weight via a facile "A2+B2+C3" approach.The structures of the hyperbranched polymers were confirmed by NMR and GPC.Their thermal,optical,and electrochemical properties of the hyperbranched polymers were also investigated.The results showed that introduction of triazatruxene units into the hyperbranched structure endowed the polymer with good thermal stability and highly amorphous properties.Photophysical investigation of PTFx revealed strong blue emission in both solution and solid states.Hyperbranched polymers with higher degree of branching and proper content of linear fluorene units exhibited better photophysical properties in terms of narrow emission spectra and relatively high quantum efficiency as well as improved thermal spectral stability.The triazatruxene branching unit also played a role in raising the HOMO energy levels relative to those of polyfluorenes that would help to improve the charge injection and transport properties.The incorporation of triazatruxene unit into hyperbranched polymers has thus explored an effective avenue for constructing optoelectronic polymers with improved functional characteristics.

Microwave-assisted synthesis of photoluminescent glutathione-capped Au/Ag nanoclusters： A unique sensor-on-a-nanoparticle for metal ions, anions, and small molecules

Even though great advances have been achieved in the synthesis of luminescent metal nanoclusters, it is still challenging to develop metal nanoclusters with high quantum efficiency as well as multiple sensing functionalities. Here, we demonstrate the rapid preparation of glutathione-capped Au/Ag nanoclusters （GS-Au/Ag NCs） using microwave irradiation and their unique sensing capacities. Compared to bare GS-Au NCs, the doped Au/Ag NCs possess an enhanced quantum yield （7.8% compared to 2.2% for GS-Au NCs）. Several characterization techniques were used to elucidate the atomic composition, particulate character, and electronic structure of the fabricated NCs. According to the X-ray photoelectron spectroscopy （XPS） and X-ray absorption near-edge structure （XANES） spectra, a significant amount of Au exists in the oxidized state as Au（I）, and the Ag atoms are positively charged. In contrast to those nanoclusters that detect only one analyte, the GS-Au/Ag NCs can be used as a versatile sensor for metal ions, anions, and small molecules. In this manner, the NCs can be regarded as a unique sensor-on-a-nanoparticle.

Microwave-assisted Solid-phase Synthesis, Biological Evaluation and Molecular Docking of Angiotensin I-converting Enzyme Inhibitors

Short peptides based on the tripeptides, Leu-Arg-Pro and Leu-Lys-Pro, were synthesized by microwave assisted solid-phase synthesis method, in order to make a search for potential inhibitors for angiotensin I-converting enzyme（ACE） with minimum side effects in the treatment of hypertension. One peptide with the sequence Leu-Arg-Pro-Phe-Phe shows the strongest inhibition towards ACE with an IC50 value of 0.26 μmol/L in vitro. The study of structure-activity relationship shows that the introduction of a bulky group into the N-terminal of this series of inhibitors may enlarge steric hindrance, resulting in the poor inhibitory activity towards ACE. The inhibitory activity decreased in turn when L-Pro, D-Pro or Ac6c was at the C-terminal respectively. The binding interaction between each of these inhibitors and testicular ACE（tACE） was performed by molecular docking. The results suggest that Leu-Arg-Pro-Phe-Phe mainly occupied the S1 subsite of tACE, and made contact with tACE via seven H-bonds. It appeared that the site on the peptide that bound with tACE was influenced by the configuration of the amino acid, L or D-form, at the C-terminal of the peptide.