Ultrasound-mediated Synthesis Research Articles

Broadband photodetectors from silane-passivated CsPbBr3 nanocrystals by ultrasound-mediated synthesis.

Perovskite nanocrystals have excellent optical properties but suffer from environmental instability and production up-scaling which limit their commercial application. Here, we report the gram-scale ultrasound-mediated synthesis of silane passivated CsPbBr3 nanocrystals using (3-aminopropyl) triethoxysilane (APTS) as the primary surface ligand surface. The surface engineering endowed the CsPbBr3@SiOR NCs with extended environmental stability, a narrow emission bandwidth and a high photoluminescence quantum yield (PLQY > 75%). Thanks to these excellent optical properties, high-efficiency lateral and vertical photodetectors were fabricated. In particular, the layered vertical photodiode composed of ITO/Ga2O3/CsPbBr3/Au exhibited a broadband photoresponse from 350-700 nm with a responsivity peaking at 44.5.1 A W-1 and specific detectivity above 1013 Jones when illuminated at 470 nm wavelength and biased at +5 V. These results correspond to the best-in-class performance perovskite nanocrystal PD and confirm the extraordinary potential of CsPbBr3@SiOR for the development of efficient optoelectronic devices.

EGCG/HP-β-CD inclusion complexes integrated into PCL/Chitosan oligosaccharide nanofiber membranes developed by ELS for fruit packaging

In this study, Epigallocatechin gallate (EGCG)/2-hydroxypropyl-β-cyclodextrin (HP-β-CD) inclusion complexes were prepared by ultrasound-mediated synthesis. EGCG/HP-β-CD and polycaprolactone (PCL)/chito-oligosaccharide (CSO) nanofiber films were rapidly prepared by electrospinning technology for fruit preservation packaging. The mean diameter of the nanofiber membrane increased from 237.11 to 552.62 nm, the water vapor permeability was enhanced, the crystallinity was decreased, and the surface was hydrophilic. Infrared spectroscopy and thermal analysis showed that hydrogen bond was formed between EGCG/HP-β-CD inclusion complex and PCL/CSO nanofibers, which improved the thermal stability of fiber films. The prepared membranes obtained long lasting release of EGCG within 240 h and showed good antibacterial activity in vitro and vivo. These results indicate that ELS has a broad application prospect in the development of postharvest antifungal nanofiber membranes.

Fast and efficient one-pot ultrasound-mediated synthesis of solid state (full color tunable) fluorescent indolizine derivatives

We report herein an efficient, fast, and sustainable method for the preparation of fluorescent indolizine derivatives under ultrasound (US) irradiation using a one-pot and multicomponent methodology. In solution, the indolizine derivatives present absorption in the UV region and fluorescence emission in the violet-to-blue region with a relatively large Stokes shift. Aggregation-induced enhanced emission (AIEE) was observed in some derivatives by fluorescence studies in water/acetone systems. Regarding this particular property, the substituents showed to play a fundamental role. In the solid state, the derivatives present full-color tunable fluorescence also tailored by the substituents. Theoretical calculations using time-dependent density functional theory were performed to investigate the photophysics of these indolizine derivatives and were able to reproduce with accuracy their more prominent electronic features.

Ultrasound-mediated synthesis of nanoporous fluorite-structured high-entropy oxides toward noble metal stabilization

SummaryHigh-entropy oxides (HEOs) are an emerging class of advanced ceramic materials capable of stabilizing ultrasmall nanoparticle catalysts. However, their fabrication still relies on high-temperature thermal treatment methodologies affording nonporous architectures. Herein, we report a facile synthesis of single-phase, fluorite-structured HEO nanocrystals via an ultrasound-mediated co-precipitation strategy under ambient conditions. Within 15 min of ultrasound exposure, high-quality fluorite-structured HEO (CeHfZrSnErOx) was generated as ultrasmall-sized particles with high surface area and high oxygen vacancy concentration. Taking advantage of these unique structural features, palladium was introduced and stabilized in the form of highly dispersed Pd nanoclusters within the CeHfZrSnErOx architecture. Neither phase segregation of the CeHfZrSnErOx support nor Pd sintering was observed under thermal treatment up to 900°C. The as-afforded Pd/CeHfZrSnErOx catalyst exhibits good catalytic performance toward CO oxidation, outperforming Pd/CeO2 of the same Pd loading, which highlights the inherent advantage of CeHfZrSnErOx as carrier support over traditional oxides.

Article Ultrasound-Mediated Synthesis of Nanoporous Fluorite-Structured High-Entropy Oxides Towards Single Atoms Stabilization

Article Ultrasound-Mediated Synthesis of Nanoporous Fluorite-Structured High-Entropy Oxides Towards Single Atoms Stabilization

Ultrasound-Mediated Synthesis of Sulfonyl Urea Derivatives and Their In Vitro Antiproliferative Activity

Ultrasound-Mediated Synthesis of Sulfonyl Urea Derivatives and Their In Vitro Antiproliferative Activity

Green Synthetic Approach: An Efficient Eco-Friendly Tool for Synthesis of Biologically Active Oxadiazole Derivatives.

Green synthetic protocol refers to the development of processes for the sustainable production of chemicals and materials. For the synthesis of various biologically active compounds, energy-efficient and environmentally benign processes are applied, such as microwave irradiation technology, ultrasound-mediated synthesis, photo-catalysis (ultraviolet, visible and infrared irradiation), molecular sieving, grinding and milling techniques, etc. Thesemethods are considered sustainable technology and become valuable green protocol to synthesize new drug molecules as theyprovidenumerous benefits over conventional synthetic methods.Based on this concept, oxadiazole derivatives are synthesized under microwave irradiation technique to reduce the formation of byproduct so that the product yield can be increased quantitatively in less reaction time. Hence, the synthesis of drug molecules under microwave irradiation follows a green chemistry approach that employs a set of principles to minimize or remove the utilization and production of hazardous toxic materials during the design, manufacture and application of chemical substances.This approach plays a major role in controlling environmental pollution by utilizing safer solvents, catalysts, suitable reaction conditions and thereby increases the atom economy and energy efficiency. Oxadiazole is a five-membered heterocyclic compound that possesses one oxygen and two nitrogen atoms in the ring system.Oxadiazole moiety is drawing considerable interest for the development of new drug candidates with potential therapeutic activities including antibacterial, antifungal, antiviral, anticonvulsant, anticancer, antimalarial, antitubercular, anti-asthmatic, antidepressant, antidiabetic, antioxidant, antiparkinsonian, analgesic and antiinflammatory, etc. This review focuses on different synthetic approaches of oxadiazole derivatives under microwave heating method and study of their various biological activities.

Facile and rapid ultrasound-mediated synthesis of spherical mesoporous silica submicron particles with high surface area and worm-like mesoporosity

Here, a facile and rapid ultrasound-mediated synthesis at ambient conditions is proposed for production of novel spherical mesoporous silica submicron particles (MSP) with high specific surface area (SSA) and high worm-like mesoporosity. A one-pot synthesis was designed to involve soft-templating with cationic surfactant cetyltrimethylammonium bromide (CTAB), application of high-power ultrasound (Us) for hydrolysis/condensation of tetraethyl orthosilicate (TEOS) in methanol/NH4OH solution and vigorous magnetic stirring. Spherical MSP with worm-like mesoporous structure were produced with average particle diameter ~545 nm, SSA ca. 1544 m2/g, total pore volume as high as 0.75 cm3/g and NLDFT pore diameter of 2.94 nm. The developed MSP hold great promise for applications e.g. H2 storage, CO2 capture, removal of Hg from gas as well as drug delivery.

Ultrasound-mediated synthesis, biological evaluation, docking and in vivo acute oral toxicity study of novel indolin-2-one coupled pyrimidine derivatives

The work reports ultrasound-mediated greener synthesis of 11 novel 3-(4-(4-chlorophenyl)-6-(substituted phenyl/heteryl)pyrimidin-2-ylimino)indolin-2-one (7a–7k) derivatives. The synthesized derivatives were evaluated for their in vitro anticancer activity against a panel of selected human cancer cell lines of breast (MCF-7), cervix (HeLa), prostate (PC-3) and lung (A-549). Among the tested compounds, 7b exhibited most promising in vitro anticancer activity against HeLa, PC-3 and A-549 with GI50 value 15.38, 19.67 and 4.37 µM, respectively. The compounds (7a–7k) were also screened for induction of apoptosis and morphological changes in cancer cells at their GI50 concentration. The treatment of HeLa, PC-3 and A549 cancer cells with 7b and treatment of MCF-7 cancer cells with 7h showed apoptosis and morphological changes such as cell shrinkage, cell wall deformation and reduced number of viable cells. The compound 7b has shown almost 5.00 times more selectivity for PC-3 cancer cell lines in comparison to the RWPE-1 normal prostate epithelial cells. Molecular docking study has been carried out, which replicates results of biological activity in cases of initial hits 7b, 7c and 7d, suggesting that these compounds have a potential to become lead molecules in the drug discovery process. In silico ADMET study was performed for predicting pharmacokinetic properties and toxicity profile of the synthesized compounds and expressed good oral drug-like behaviour. An in vivo acute oral toxicity study was performed using Swiss albino mice for the most active compounds 7b and 7c, and results indicate that the compounds are non-toxic in nature.

Novel O‐Alkylated Chromones as Antimicrobial Agents: Ultrasound Mediated Synthesis, Molecular Docking and ADME Prediction

In the development of novel antimicrobial agents, we synthesized novel O‐alkylated chromones 4a–f by ultrasound‐assisted method. The synthesized compounds were characterized by IR, 1H NMR, 13C NMR, MS, and elemental analysis. All compounds were assessed in vitro for their efficacy as antimicrobial agents against four bacteria (Staphylococcus aureus, Bacillus subtilis, Escherichia coli, Pseudomonas aeruginosa) and three fungi (Candida albicans, Candida glabrata, Candida tropicalis). In particular, compounds 4a, 4b, 4d, 4e, and 4f exhibited potent antimicrobial activity. Molecular docking study was used to rationalize binding interaction at the active site, and the result showed good binding interaction. The compounds were also processed for in silico ADME prediction, and the result showed that compounds could be exploited as an oral drug candidate.

Molecular sieves promoted, ultrasound-mediated synthesis, biological evaluation and docking study of 3-(5-substituted-1,3,4-thiadiazol-2-ylimino)indolin-2-ones as a potential anticonvulsant agents

In this work, the combined use of ultrasonic energy and molecular sieves was investigated for synthesis of 3-(5-substituted-1,3,4-thiadiazol-2-ylimino)indolin-2-one derivatives 5(a–j). The equimolar quantities of 5-substituted-1,3,4-thiadiazol-2-amine and isatin were sonicated in the presence of activated molecular sieves 3 A at a temperature of 50 °C and at a frequency 20 kHz, and higher yields (73–92 %) and faster reaction times (43–75 min) were obtained when ultrasonic irradiation was used in comparison with conventional methods. The synthesized compounds were evaluated for anticonvulsant (MES and sc-PTZ model) and behavioral activity (actophotometer) in mice. The compounds 5b, 5i and 5j have shown protection against MES model at 0.5- and 4-h period at dose level of 100 mg/kg, while the compound 5c showed protection against sc-PTZ model at the same dose level. To exploit the mode of action of the synthesized compounds, docking study against sodium channel receptor was performed and the results revealed good binding interactions with the receptor. ADME properties of synthesized compounds were also analyzed and showed potential to develop as good oral drug candidates.

Ultrasound-Mediated Synthesis of 2,4,6-Triaryl-Pyridines Using MgAl2O4 Nanostructures

Ultrasound-accelerated organic chemical reactions have been increasingly developed by researchers across the globe for the synthesis of organic compounds. Ultrasound irradiation offers an alternative energy source for organic synthesis which are ordinarily accomplished by heating. Ultrasound- mediated reactions proceed by the formation, growth and collapse of acoustic bubbles in the reaction medium. These directly help in shortening the time span of reactions and increasing the yield of products [1]. The pyridine ring system is present in various natural compounds, and many pyridines exhibit a board range of biological activities [2]. Due to their π-stacking ability, some pyridine derivatives are used in supramolecular chemistry [3]. Recently, these heterocyclic compounds have also been evoked considerable attention as these endowed with wide range of pharmaceutical activities such as anticovulsant, antimalarial, anesthetic, vasodilator, and antiepileptic and agrochemicals such as pesticidial, fungicidal and herbicidal [4,5]. Therefore, it has attracted continuous interest to develop procedures for the synthesis of 2,4,6triarylpyridines, Krohnke pyridines. Since Krohnke's original report on the preparation of 2,4,6-triarylpyridines [6], there has been a plethora of research targeting their syntheses [7-12]. Recently, much effort has been devoted to developing more efficient protocols for the synthesis of 2,4,6-triarylpyridines, for example solid-phase synthesis [7], one-pot synthesis under microwave irradiation [8], solvent-free reaction between acetophenones, benzaldehydes, and ammonium acetate in the presence of various catalyst such as I2 [9], heteropolyacid [10], HClO4-SiO2 [11] and ionic liquid [12]. However, many of these processes suffer from drawbacks such as long reaction time, expensive catalyst, undesired side products in reaction with harsh reagents, special care in handling and storing the reagents, cumber some product isolation procedure and environmental pollution. Therefore, a need still exists for further development of versatile reaction conditions in synthesis of 2,4,6-triarylpyridine using an efficient, reusable, inexpensive, eco-friendly, green, great and selectivity catalyst. In recent years, nanostructures have emerged as powerful catalysts in various organic synthesis such as cobalt nanoparticles for synthesis of 1,4Dihydropyridines [13], nanocrystalline MgO for synthesis of 2,4,5-trisubstituted imidazole derivatives [14], silica nanoparticles for preparation highly substituted pyridines [15] and ZnO nano powder for the preparation of 2,4,6-triaryl pyridines

Ultrasound-mediated synthesis of 4-substituted 1,4-dihydropyridine-3,5-dicarboxylates catalyzed by 1-carboxymethyl-3-methylimidazolium tetrafluoroborate under solvent free condition

4-Substituted 1,4-dihydropyridine-3,5-dicarboxylates (4) have been synthesized by the solvent-free reaction of aldehyde, methyl propiolate and ammonium carbonate catalyzed by ionic liquid 1-carboxymethyl-3-methylimidazolium tetrafluoroborate under ultrasonic irradiation. The effects of changes in the ultrasonic power, temperature, catalysts and reactants on the synthesis of 4-substituted 1,4-dihydropyridine-3,5-dicarboxylates (4) are discussed. With the optimized reaction conditions, various aldehydes were used to synthesize 1,4-dihydropyridines (4) under the influence of ultrasound irradiation. Compared with the conventional thermal methods, the remarkable advantages of this method are the simple experimental procedure, shorter reaction time (2–10min) and high yield of product (76–95%). Furthermore, the green catalytic system can be recycled specific times without significantly decreasing the yields and reaction rates.

Ultrasound-Mediated Synthesis of 3,4-Dihydropyrimidin-2-(1H)-Ones (or Thiones) with NaHSO4·H2O

A fast and efficient Biginelli synthesis of 3,4-dihydropyrimidin-2-(1H)-ones (or thiones) by the reaction of aromatic aldehydes, β-dicarbonyls, and urea/thiourea using NaHSO4·H2O/ultrasound system is presented. The reactions were carried out in refluxing n-hexane/CH3CN (2.5:0.5 mL) to afford the products in excellent yields.

Ultrasound-mediated synthesis of phenothiazine derivatives and their in vitro antibacterial and antioxidant studies

A series of N′-((10-alkyl-10H-phenothiazin-3-yl)methylene)benzohydrazide have been synthesized via condensation of 10-alkyl-10H-phenothiazine-3-carbaldehyde with different heterocyclic acetohydrazides. The reactions were carried out under both conventional and ultrasonic irradiation conditions. In general, improvement in rates and yields were observed when reactions were carried out under sonication compared to classical synthetic conditions. Structures of all the newly synthesized compounds were characterized by IR, 1H NMR, 13C NMR, and mass spectra. Antibacterial activities of the synthesized compounds were studied against bacterial strains Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa, Bacillus cereus, and Klebsiella pneumonia. The free radical scavenging activities of synthesized compounds were screened for in vitro antioxidant activity.

Ultrasound-mediated synthesis of N,N-bis(phenacyl)aniline under solvent-free conditions.

An efficient method for the synthesis of N,N-bis(phenacyl)anilines was developed via smooth condensation of anilines with α-bromoacetophenones in the presence of sodium carbonate as acid acceptor and polyethylene glycol 400 (PEG 400) as catalyst at room temperature under solvent-free conditions by using 350 W ultrasound irradiation. In addition to experimental simplicity, the main advantages of the procedure are mild conditions, short reaction times (30–45 min), and high yields (73–83 %).Graphical

Lipase catalyzed ultrasonic synthesis of poly-4-hydroxybutyrate-co-6-hydroxyhexanoate

Four different lipases were compared for ultrasound-mediated synthesis of the biodegradable copolymer poly-4-hydroxybutyrate-co-6-hydroxyhexanoate. The copolymerization was carried out in chloroform. Of the enzymes tested, Novozym 435 exhibited the highest copolymerization rate, in fact the reaction rate was observed to increase with about 26-fold from 30 to 50°C (7.9×10−3Ms−1), sonic power intensity of 2.6×103Wm−2 and dissipated energy of 130.4Jml−1. Copolymerization rates with the Candida antarctica lipase A, Candida rugosa lipase, and Lecitase Ultra™ were lower at 2.4×10−4, 1.3×10−4 and 3.5×10−4Ms−1, respectively. The catalytic efficiency depended on the enzyme. The efficiency ranged from 4.15×10−3s−1M−1 for Novozym 435–1.48×10−3s−1M−1 for C. rugosa lipase. Depending on the enzyme and sonication intensity, the monomer conversion ranged from 8.2% to 48.5%. The sonication power, time and temperature were found to affect the rate of copolymerization. Increasing sonication power intensity from 1.9×103 to 4.5×103Wm−2 resulted in an increased in acoustic pressure (Pa) from 3.7×108 to 5.7×108Nm−2 almost 2.4–3.7 times greater than the acoustic pressure (1.5×108Nm−2) that is required to cause cavitation in water. A corresponding acoustic particle acceleration (a) of 9.6×103–1.5×104ms−2 was calculated i.e. approximately 984–1500 times greater than under the action of gravity.

Convenient ultrasound-mediated synthesis of 1,4-diazabutadienes under solvent-free conditions

An ultrasound-assisted preparation of 1,4-diazabutadienes via smooth condensation of diketones with amines under solvent-free conditions is described. The generality of this method was examined by the synthesized N, N′-diaryl- and N, N′-dialkyl-1,4-diazabutadiene derivatives. In addition to experimental simplicity, the main advantages of the procedure are mild conditions, short reaction time (2–15 min) and high yields (71–98%).

Ultrasound‐mediated synthesis of camphoric acid‐based chiral salens for the enantioselective trimethylsilylcyanation of aldehydes

New chiral salen ligands were prepared by the ultrasound-irradiated condensation of optically active (1R, 3S)-1,2,2-trimethyl-1,3-diaminocyclopentane with aromatic 1-hydroxyaldehydes. The ultrasound-mediated process is more convenient due to shorter reaction times, energy economy, and easier isolation of the products. The in situ formed Ti(IV)(salen) complexes, evaluated as catalysts in the enantioselective trimethylsilylcyanation of benzaldehyde, were found to be efficient for this process, originating the corresponding product in high yields (72-99%) and selectivities of up to 79%. The lowest energy transition states were determined by computational studies. These results were in qualitative agreement with the experimentally observed ones.

ChemInform Abstract: Ultrasound‐Mediated Synthesis and Mass Spectrometric Fragmentation of Dimethyl‐Substituted 1,2‐Diphenylethanols, Convenient Dimethylstilbene Precursors.

ChemInformVolume 18, Issue 46 Isocyclic Compounds ChemInform Abstract: Ultrasound-Mediated Synthesis and Mass Spectrometric Fragmentation of Dimethyl-Substituted 1,2-Diphenylethanols, Convenient Dimethylstilbene Precursors. I. C. BURKOW, I. C. BURKOW Dep. Chem., Univ. Tromso, N-9001 Tromso, NorwaySearch for more papers by this authorL. K. SYDNES, L. K. SYDNES Dep. Chem., Univ. Tromso, N-9001 Tromso, NorwaySearch for more papers by this authorD. C. N. UBEDA, D. C. N. UBEDA Dep. Chem., Univ. Tromso, N-9001 Tromso, NorwaySearch for more papers by this author I. C. BURKOW, I. C. BURKOW Dep. Chem., Univ. Tromso, N-9001 Tromso, NorwaySearch for more papers by this authorL. K. SYDNES, L. K. SYDNES Dep. Chem., Univ. Tromso, N-9001 Tromso, NorwaySearch for more papers by this authorD. C. N. UBEDA, D. C. N. UBEDA Dep. Chem., Univ. Tromso, N-9001 Tromso, NorwaySearch for more papers by this author First published: November 17, 1987 https://doi.org/10.1002/chin.198746159Read the full textAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article. Volume18, Issue46November 17, 1987 RelatedInformation