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Wood ash is a naturally alkaline derived substance containing organic and inorganic constituents. This study investigates the catalytic activity of wood ash as a heterogeneous catalyst for the synthesis of benzochromene derivatives. Several wood ash catalysts, comprising calcium- and potassium-rich carbonates, were prepared from different natural resources under various combustion temperatures. The prepared catalysts were characterized by Fourier transform infrared, scanning electron microscopy, energy dispersive X-ray analysis, transmission electron microscopy, and X-ray diffraction techniques. Catalytic efficiency of the resultant catalysts was tested in the synthesis of benzochromene derivatives. The experimental studies clarified that the catalyst prepared at 850 °C could efficiently expedite the formation of three-component synthesis of benzochromene derivatives in water at 80 °C with high yields. Indeed, alkali, alkaline metal, and metal oxides such as Al2O3, SiO2, MgO, CaO, and Fe2O3, are widely utilized as both catalyst and catalyst support in the heterogeneous catalytic processes. The prepared wood ash catalysts (possessing metal oxides, e.g., CuO, Al2O3, SiO2, and CaO) could effectively prompt the electrophilic activity of the carbonyl groups during the nucleophilic attack intermediate, enhancing the efficiency of the reactions.
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The human population is generally subjected to diverse pollutants and contaminants in the environment like those in the air, soil, foodstuffs, and drinking water. Therefore, the development of novel purification techniques and efficient detection devices for pollutants is an important challenge. To date, experts in the field have designed distinctive analytical procedures for the detection of pollutants including gas chromatography/mass spectrometry and atomic absorption spectroscopy. While the mentioned procedures enjoy high sensitivity, they suffer from being laborious, expensive, require advanced skills for operation, and are inconvenient to deploy as a result of their massive size. Therefore, in response to the above-mentioned limitations, electrochemical sensors are being developed that enjoy robustness, selectivity, sensitivity, and real-time measurements. Considerable advancements in nanomaterials-based electrochemical sensor platforms have helped to generate new technologies to ensure environmental and human safety. Recently, investigators have expanded considerable effort to utilize polymer nanocomposites for building the electrochemical sensors in view of their promising features such as very good electrocatalytic activities, higher electrical conductivity, and effective surface area in comparison to the traditional polymers. Herein, the first section of this review briefly discusses the most important methods for polymer nanocomposites synthesis, such as in situ polymerization, direct mixing of polymer and nanofillers (melt-mixing and solution-mixing), sol-gel, and electrochemical methods. It then summarizes the current utilization of polymer nanocomposites for the preparation of electrochemical sensors as a novel approach for monitoring and detecting environmental pollutants which include heavy metal ions, pesticides, phenolic compounds, nitroaromatic compounds, nitrite, and hydrazine in different mediums. Finally, the current challenges and future directions for the polymer nanocomposites-based electrochemical sensing of environmental pollutants are outlined.
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Synthesis of bioactive heterocyclic compounds having effective biological activity is an essential research area for wide-ranging applications. In this study, a conventional methodology has been developed for the synthesis of a series of new 3-mercapto-1,2,4-triazole derivatives 4a-f. The purity and structure of the synthesized molecules were confirmed by 1H NMR, 13C NMR and elemental analysis. In addition, the prepared compounds were screened for their anti-proliferative activity against three human cancer cell lines including A549 (lung cancer), MCF7 (breast cancer) and SKOV3 (ovarian cancer) using MTT reduction assay. All the tested compounds demonstrated remarkable cytotoxic activity with IC50 values ranging from 3.02 to 15.37 µM. The heterocyclic compound bearing 3,4,5-trimethoxy moiety was found to be the most effective among the series displaying an IC50 of 3.02 µM specifically against the ovarian carcinoma cancer cell line (SKOV3). Moreover, Annexin V-FITC/propidium iodide staining assay indicated that this compound can induce apoptosis in SKOV3 cells. Furthermore, cell cycle assay showed a significant cell cycle arrest at the G2/M phase in a dose-dependent manner for this compound. The molecular docking results was showed binding modes of potent compound 4d perfectly corroborated the suggestion of binding to the colchicine site. The entire results conclude that 3-mercapto-1,2,4-triazole derivatives can be synthesized by a green method for biological and pharmacological applications. New analogs of 3-mercapto-1,2,4-triazole potential derivatives for anti-proliferative activity were synthesized. Cytotoxic activity of all synthesized compounds was evaluated against tree human cancer cell lines: lung (A549), breast (MCF7) and ovarian (SKOV3).
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Antineoplásicos/síntesis química , Antineoplásicos/farmacología , Triazoles/síntesis química , Triazoles/farmacología , Células A549 , Apoptosis/efectos de los fármacos , Puntos de Control del Ciclo Celular/efectos de los fármacos , División Celular/efectos de los fármacos , Línea Celular Tumoral , Proliferación Celular/efectos de los fármacos , Ensayos de Selección de Medicamentos Antitumorales/métodos , Fase G2/efectos de los fármacos , Compuestos Heterocíclicos/síntesis química , Compuestos Heterocíclicos/farmacología , Humanos , Células MCF-7 , Simulación del Acoplamiento Molecular/métodos , Relación Estructura-ActividadRESUMEN
Aims & Objective: An efficient procedure for the synthesis of pyrido[2,1-a]isoquinoline derivatives in excellent yields was investigated using catalyst-free multicomponent reaction of phthaladehyde, methylamine, activated acetylenic compounds, alkyl bromides and triphenylphosphine in water under ultrasonic irradiation at room temperature. In addition, Diels- Alder reactions of pyrido[2,1-a]isoquinoline derivatives with activated acetylenic compounds under ultrasonic irradiation are investigated in two procedures. The advantages of this procedure compared to report methods are short time of reaction, high yields of product, easy separation of product, clean mixture of reaction and green media for performing reaction. In addition, because of having isoquinoline core in synthesized compounds, in this research antioxidant activity of some synthesized compounds was studied. MATERIALS AND METHODS: To a stirred mixture of phthalaldehyde 1 (2 mmol) and methylamine 2 (2 mmol) in water (3 mL) under ultrasonic irradiation was added to activated acetylenic compounds 4 after 20 min. Alkyl bromide 3 and triphenylphosphine 5 react in another pot in water (3 mL) under ultrasonic irradiation for 15 min. After this time, this mixture was added to the first pot. After completion of the reaction, the solid residue was separated by filtration and washed with Et2O to afforded pure title compound 6. RESULTS: In this work, generation of pyrido[2,1-a]isoquinoline derivatives 6 are performed using phthalaldehyde 1, methylamine 2, α-halo substituted carbonyls 3, activated acetylenic compounds 4 and triphenylphosphine 5 in water under ultrasonic irradiation condition at room temperature in excellent yield at short time. CONCLUSION: In summary, multicomponent reaction of phthaladehyde, methylamine, activated acetylenic compounds, alkyl bromides and triphenylphosphine in water under ultrasonic irradiation at room temperature produced pyrido[2,1-a]isoquinoline derivatives in excellent yields. Also, Diels-Alder reaction of pyrido[2,1-a]isoquinoline derivatives with activated acetylenic compounds and triphenylphosphine under ultrasonic irradiation is investigated in two procedures. Also, the antioxidant activities of 6a, 6c, 6g and 6i were evaluated by DPPH radical scavenging and ferric reducing power analyzes. The compounds 6a exhibit excellent DPPH radical scavenging activity and FRAP compared to synthetic antioxidants BHT and TBHQ. The chief benefits of our method are high atom economy, green reaction conditions, higher yield, shorter reaction times, and easy work-up, which agree with some principles of green chemistry.
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Antioxidantes/síntesis química , Isoquinolinas/síntesis química , Aldehídos/química , Alquinos/química , Antioxidantes/farmacología , Bromuros/química , Catálisis , Compuestos Férricos/química , Depuradores de Radicales Libres/química , Tecnología Química Verde , Humanos , Isoquinolinas/farmacología , Metilaminas/química , Compuestos Organofosforados/química , Oxidación-Reducción , UltrasonidoRESUMEN
Hydrogels were synthesized by a copolymerization reaction of nanofibrillated cellulose (CNF) with acrylic acid (AA) and acrylamide (AM) and N,N-methylene-bis-acrylamide (MBA) as a cross-linker and their absorption performance as a function of composition was determined. Hydrogels with 4% by weight CNF had swelling of about 250 g/g and with 7% CNF about 200 g/g for water. Thermodynamic and kinetic studies of the reaction pathways and the electronic properties of the cellulose and monomers were investigated through density functional theory calculations. Thermodynamic investigations revealed that the radical formation of cellulose that initiates the hydrogel process can occur through the breaking of the homolytic covalent bonds C6-OH and C3-OH. The results show that the reaction of CNF with monomers is thermodynamically favorable in the decreasing order of AM, AA, and MBA. The kinetic study also indicates that the reaction kinetics of CNF with AM is faster than with AA which is much faster than with MBA. Overall, this study has elucidated some of the key chemical characteristics that impact the derivatization of nanocellulose structures to produce advanced renewable bioproducts.
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Celulosa/química , Hidrogeles/síntesis química , Nanofibras/química , Hidrogeles/química , Concentración de Iones de Hidrógeno , Cinética , Polimerizacion , Temperatura , TermodinámicaRESUMEN
BACKGROUND: There are a number of protocols for Ullmann coupling-type S-arylation reactions, many of them suffer from the use of homogenous and often corrosive catalyst, cumbersome workup procedures, and long reaction times. Besides, many of these reagents are expensive and non-recoverable, leading to the generation of a large amount of toxic waste particularly when large-scale applications are considered. OBJECTIVE: The aim of this study was to prepare a new Pd catalyst bonded on the surface of zeolite as a heterogeneous catalyst. METHODS: A heterogeneous palladium catalyst has been prepared by immobilizing Pd ions on Clinoptilolite. This novel developed heterogeneous catalyst was thoroughly examined for Ullmann coupling-type S-arylation reaction using different bases, solvents and 0.003 mg of the catalyst. The structural and morphological characterizations of the catalyst were carried out using XRD, TGA, BET and TEM techniques. RESULTS: Highly efficient heterogeneous palladium catalyst has been developed by immobilizing Pd ions on Clinoptilolite, as one of the most abundant naturally occurring zeolites for Ullmann Sarylation. By using this method, we provide an efficient way to a wide variety of substituted thiolic compounds. Moreover, the catalyst is easily recovered using simple filtration and reused for 5 consecutive runs. CONCLUSION: In this effort, we developed a new Pd catalyst bonded on the surface of zeolite as a substrate to prepare the heterogeneous catalyst. We demonstrate that this novel catalyst offers reliable and convincing data that may offer a valuable application in further developing the science and technology of Ullmann reaction protocols and allied industries. Additionally, the catalyst was reusable and kept its high activities over a number of cycles.
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Complejos de Coordinación/química , Hidrocarburos Halogenados/síntesis química , Paladio/química , Compuestos de Sulfhidrilo/síntesis química , Zeolitas/química , Catálisis , Hidrocarburos Halogenados/química , Estructura Molecular , Tamaño de la Partícula , Compuestos de Sulfhidrilo/química , Propiedades de SuperficieRESUMEN
This study is on current developments concerning ferrocene (FC) and its derivatives on the basis of electrochemical biosensors and sensors. The distinct physiochemical characteristics of FC have enabled the development of new sensor devices, specifically electrochemical sensors. Several articles have focused on the implementation of FC as an electrode constituent while discussing its electrochemical behavior. Furthermore, typical FC-design-based biosensors and sensors are considered as well as practical examples. The favorable design of FC-based biosensors and general sensors needs adequate control of their chemical and physical characteristics in addition to their surface immobilization and functionalization.
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Capacitors allow extremely fast charge and discharge operations, which is a challenge faced by recent metal-ion batteries despite having highly improved energy densities. Thus, combined type electric energy storage devices that can integrate high energy density and high power density with high potentials, can overcome the shortcomings of the current metal-ion batteries and capacitors. However, the limited capacities of cathode materials owing to the barren redox reactions are regarded as an obstacle for the development of future high-performance hybrid metal-ion capacitors. In this study, we demonstrate the redox-reaction-rendering effect of the much overlooked lanthanide elements when used as the cathode of lithium-ion capacitors using the mesoporous carbon (MC) as a matrix material. Consequently, these lanthanide elements can effectively enrich the redox reaction, thus improving the capacity of the matrix materials by more than two times. Typically, the Gd-elemental decoration of MC surprisingly enhances the capacity by almost two times as compared with the underacted MC. Furthermore, the La nanoparticles (NPs) decoration depicts the same behavior. Evident redox peaks were formed on the original rectangular cyclic voltammetry (CV) curves. This study provides the first example of embedding lanthanide elements on matrix materials to enrich the desired redox reactions for improving the electrochemical performances.
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The present investigation examines a sensitive electrochemical technique to detect desipramine through Fe3O4/CuO nanoparticles (NPs). Fe3O4/CuO NPs were synthesized via a coprecipitation procedure, and the products were characterized via energy disperse spectroscopy, X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and vibrating sample magnetometer. The voltage-current curve and differential pulse voltammetry examinations of Fe3O4/CuO-modified screen-printed electrode (Fe3O4/CuO/SPE) were followed by the determination of electro-catalytic activities toward desipramine oxidation in a phosphate buffer solution (pH = 7.0). In addition, the value of diffusion coefficient (D = 3.0 × 10-6 cm2 s-1) for desipramine was calculated. Then, based on the optimum conditions, it was observed that the currents of the oxidation peak were linearly proportionate to the concentration of desipramine in the broad range between 0.08 and 400.0 µM and LOD of 0.03 µM (S/N = 3). Finally, our new sensor was successfully utilized to detect desipramine in the real samples, with reasonable recovery in the range of 97.2% to 102.7%.
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Scientists have categorized conductive polymers as materials having strongly reversible redox behavior and uncommon combined features of plastics and metal. Because of their multifunctional characteristics, e.g., simplistic synthesis, acceptable environmental stability, beneficial optical, electronic, and mechanical features, researchers have largely considered them for diverse applications. Therefore, their capability of catalyzing several electrode reactions has been introduced as one of their significant features. A thin layer of the conducting polymer deposited on the substrate electrode surface can augment the electrode process kinetics of several solution species. Such electrocatalytic procedures with modified conducting polymer electrodes can create beneficial utilization in diverse fields of applied electrochemistry. This review article explores typical recent applications of conductive polymers (2016-2020) as active electrode materials for energy storage applications, electrochemical sensing, and conversion fields such as electrochemical supercapacitors, lithium-ion batteries, fuel cells, and solar cells.
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Potassium fluoride impregnated on clinoptilolite nanoparticles (KF/CP NPs) was investigated as an efficient solid base catalyst for multicomponent condensation reaction. A broad range of aromatic aldehydes and enolizable compounds were condensed with 2-naphthol or 4-hydroxycumarine. The reaction was carried out under a solvent-free condition to give the corresponding benzoxanthene and pyrano [3,2-c]chromene derivatives in high yields. The low cost and availability of catalyst, novel and green procedure makes this strategy more useful for the preparation of tetrahydrobenzo[a]-xanthene-11-one and pyrano [3,2-c]chromene derivatives.
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Communicated by Ramaswamy H. Sarma.
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Atropina/química , Sistemas de Liberación de Medicamentos , Frecuencia Cardíaca/efectos de los fármacos , Nanotubos de Carbono/química , Adsorción/efectos de los fármacos , Atropina/farmacología , Calcio/química , Gases/química , Humanos , Teoría Cuántica , Solventes/químicaRESUMEN
Starch nanocrystal was prepared using weak sulfuric acid hydrolysis at 40 °C. Transmission electron micrographs of dilute suspensions of starch nanocrystals showed round particles with a diameter ranging from 20 to 40 nm. SEM of freeze dried samples showed separated particles between 40 and 100 nm and confirmed production of starch nano particles. XRD patterns obtained for the prepared nanostarch and raw starch sample showed no special pattern of crystallinity for starch sample. Extracted nanostarch showed pattern of crystallinity with the peaks at Bragg angles (2θ) at about 15° and 23°, and a doublet at 17° and 18°. The crystalline structure of prepared sample was A-type. FTIR spectra confirmed the particles oxidation. Nano silver particle was precipitated on the starch nano particle. UV spectra confirmed the presence of silver particle on the starch particles. Inhibitions tests of nanostarch bearing nano silver on three types of bacteria was investigated. The inhibition test results were 25 µg/mL for S. aureus, and S. typhi, and 12.5 µg/mL for E. coli.
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A high-quality method for one-pot biosynthesis of silver nanoparticles (AgNPs) using onion extracts as reductant and stabilizer is reported. The synthesized AgNPs were characterized by ultraviolet-visible spectroscopy (UV-Vis), X-ray powder diffraction (XRD), and transmission electron microscopy (TEM). UV-Vis spectroscopy results showed that the AgNP absorption band was located at a peak of 397 nm in aqueous solution. Both XRD and TEM results confirmed that the AgNPs were mainly spherical with average diameters of 6.0 nm by TEM and about 5.3-10.2 nm calculated using XRD data. The ability of AgNPs to reduce charge transfer resistance was also investigated using electrochemical impedance spectroscopy. Finally, the effect of synthesized NPs on ascorbic acid signal was investigated by square wave voltammetry. The peak current of square wave voltammograms of ascorbic acid increased linearly with its concentration in the range of 0.4-450.0µM. The detection limit for ascorbic acid was 0.1µM.
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Cebollas , Ácido Ascórbico , Electrodos , Nanopartículas del Metal , Extractos Vegetales , Plata , Espectrofotometría UltravioletaRESUMEN
An efficient and selective synthesis of substituted chromene derivatives via three-component reaction of 4-hydroxycoumarin or 1,3-dicarbonyl compounds, activated acetylenic compounds and N-nucleophiles is described. The reaction was conducted under solvent-free conditions at 70°C using potassium fluoride impregnated on natural zeolite as a cheap and available solid base. The procedure has several advantages involving selectivity, excellent yields and a convenient work-up method.
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Benzopiranos/química , Benzopiranos/síntesis química , Nanoestructuras/química , Zeolitas/química , 4-Hidroxicumarinas/química , Acetileno/química , Catálisis , Técnicas Químicas Combinatorias , Ensayos Analíticos de Alto Rendimiento , Estructura Molecular , Quinolinas/químicaRESUMEN
A series of furo[3,2-c]coumarin derivatives 1a-d were synthesized and evaluated for their antiproliferative activity against MCF-7 breast and HCT-15 colon cancer cell lines using Sulfo-rhodamine B (SRB) assay. Compounds 1b and 1d showed higher antiproliferative activity than 1a and 1c. UV-Vis spectroscopy was used for DNA and BSA-binding affinity of the compounds 1b and 1d and gave overall affinity constants of K1b-DNA=8.1×10(3) M(-1), K1d-DNA=1.1×10(4) M(-1), K1b-BSA=5.1×10(4) M(-1), and K1d-BSA=7.6×10(4) M(-1). Our findings could provide new evidence showing the relationship between the chemical structure and anticancer activity of these new coumarin analogs.
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Antineoplásicos/síntesis química , Cumarinas/química , Antineoplásicos/metabolismo , Antineoplásicos/farmacología , Sitios de Unión , Línea Celular Tumoral , Proliferación Celular/efectos de los fármacos , Cumarinas/metabolismo , Cumarinas/farmacología , ADN/química , ADN/metabolismo , Humanos , Cinética , Células MCF-7 , Simulación del Acoplamiento Molecular , Unión Proteica , Estructura Terciaria de Proteína , Albúmina Sérica Bovina/química , Albúmina Sérica Bovina/metabolismoRESUMEN
In the present study, we report electrosynthesis of 4,5-bis(4-chloroanilino)-1,2-benzendiol (BCB) and its application as a selective electrochemical mediator at a surface of carbon paste electrode (CPE) modified ZnO/CNTs nanocomposite as a simple and rapid voltammetric sensor. The sensor showed an efficient catalytic activity for the electro-oxidation of glutathione (GSH), which leads to a lowered overpotential by more than 203 mV compared to unmodified carbon paste electrode. For the mixture containing GSH, nicotinamide adenine dinucleotide (NADH) and folic acid (FA), the electrooxidation signals were well separated. The square wave voltammetry (SWV) currents increased linearly with their concentration at the ranges of 0.006-161, 1.0-650 and 3.0-700 µM, respectively with the detection limits of 0.002, 0.3 and 1.0 µM. Finally, the electrode was successfully applied for the voltammetric determination of analytes in real samples with satisfactory results.
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Técnicas Electroquímicas/instrumentación , Ácido Fólico/análisis , Glutatión/análisis , NAD/análisis , Nanotecnología , Límite de Detección , Microscopía Electrónica de Transmisión , Oxidación-Reducción , Reproducibilidad de los ResultadosRESUMEN
The electrochemistry of bisphenol A (BPA) was studied by voltammetric methods at a surface of carbon paste electrode modified by a ZnO/CNTs nanocomposite and room-temperature ionic liquid of 1,3-dipropylimidazolium bromide. The ratio of ZnO/CNTs and ionic liquid (IL) on the surface of the electrode has to be controlled carefully because the charging currents. The anodic peaks of BPA and Sudan I in their mixture can be well separated. At pH 7.0 the two peaks are separated ca. 0.47 and 0.70 V, respectively; hence BPA can be determined in the presence of Sudan I and more than 8.7 times current excess of BPA. The peaks current of square wave voltammograms (SWV) of BPA and Sudan I increased linearly with their concentration in the ranges of 0.002-700 µmol L(-1)BPA and 0.2-800 µmol L(-1) Sudan I. The detection limits for BPA and Sudan I were 9.0 nmol L(-1) and 80 nmol L(-1), respectively. The modified electrode has been successfully applied for the assay of BPA in food samples. This study provides a simple and easy approach to selectively detect BPA in the presence of Sudan I.
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Compuestos de Bencidrilo/química , Líquidos Iónicos/química , Fenoles/química , Óxido de Zinc/química , Electroquímica , Electrodos , Análisis de los Alimentos , Nanocompuestos , NaftolesRESUMEN
1-(6-Hydroxy-2-isopropenyl-1-benzofuran-5-yl)-1-ethanone (1), isolated from the roots of Petasites hybridus L., and a series of synthetic benzoxazepine derivatives of compound 1 (2-6) were evaluated for their immunomodulatory effects. The compounds were evaluated for their effects on the respiratory burst of human whole blood and isolated human polymorphonuclear leukocytes (PMNs) using luminol- and lucigenin-based chemiluminescence (CL) assays, and their effect on chemotactic migration of PMNs was assessed using the Boyden chamber technique. Compound 1 exhibited stronger inhibition than acetylsalicylic acid (ASA) on luminol-enhanced CL of PMNs. It also inhibited PMN chemotaxis with an IC50 value comparable to that of ibuprofen. Of the compounds tested, 5 was the most effective in inhibiting luminol-enhanced CL and also strongly inhibited lucigenin-enhanced CL with IC50 values lower than that of ASA. Compound 2 was the most active in inhibiting migration of PMNs and was five times stronger than ibuprofen. The results suggest that compound 1 and its synthesized benzoxazepine derivatives, especially compounds 2 and 5, were able to modulate the innate immune response of phagocytes at different steps, emphasizing their potential as leads for the development of new immunomodulatory agents.
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Benzofuranos/farmacología , Factores Inmunológicos/farmacología , Petasites/química , Adulto , Benzofuranos/síntesis química , Benzofuranos/química , Quimiotaxis/efectos de los fármacos , Humanos , Factores Inmunológicos/química , Neutrófilos/efectos de los fármacos , Neutrófilos/inmunología , Especies Reactivas de Oxígeno/metabolismo , Adulto JovenRESUMEN
The bark of Litsea costalis affords two new compounds named 4,4'-diallyl-5,5'-dimethoxy-[1,1'-biphennyl]-2,2'-diol, biseugenol A (1) and 2,2'-oxybis (4-allyl-1-methoxybenzene), biseugenol B (2) along with two known compounds (3-4), namely 5-methoxy-2-Hydroxy Benzaldehyde (3), and (E)-4-styrylphenol (4). The structures of 1 and 2 were determined using 1D and 2D NMR data. Also, the IR and NMR data were combined with quantum chemical calculations in the DFT approach using the hybrid B3LYP exchange-correlation function to confirm the structures of the compounds. Compounds showed fairly potent anticancer activity against cell lines and antioxidant (DPPH).