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1.
Drug Dev Ind Pharm ; 50(1): 23-35, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38079333

RESUMO

OBJECTIVE: This study aimed to develop a mixed polymeric micelle formulation incorporating candesartan cilexetil (CAND) drug to enhance its oral bioavailability for the better treatment of hypertension. METHODS: A Box-Behnken design was utilized to optimize the CAND-incorporated mixed polymeric micelles formulation (CAND-PFLC) consisting of Pluronics (P123 and F68) and lecithin (LC). The optimized CAND-PFLC micelles formulation was characterized for size, shape, zeta potential, polydispersity index (PDI), and entrapment efficiency (%EE). An in vitro release study, ex vivo permeability investigation, and an in vivo pharmacokinetic analysis were carried out to evaluate the performance of the formulation. RESULTS: The optimized CAND-PFLC micelles formulation demonstrated a spherical shape, a particle size of 44 ± 2.03 nm, a zeta potential of -7.07 ± 1.39 mV, a PDI of 0.326 ± 0.06, and an entrapment efficiency of 87 ± 3.12%. The formulation exhibited excellent compatibility, better stability, and a noncrystalline nature. An in vitro release study revealed a faster drug release of 7.98% at gastric pH in 2 hrs and 94.45% at intestinal pH within 24 hrs. The ex vivo investigation demonstrated a significantly enhanced permeability of CAND, with 94.86% in the micelle formulation compared to 9.03% of the pure drug. In vivo pharmacokinetic analysis showed a 4.11-fold increase in oral bioavailability of CAND compared to the marketed formulation. CONCLUSION: The CAND-PFLC mixed micelle formulation demonstrated improved performance compared to pure CAND, indicating its potential as a promising oral drug delivery system for the effective treatment of hypertension.


Assuntos
Benzimidazóis , Compostos de Bifenilo , Hipertensão , Micelas , Tetrazóis , Humanos , Poloxâmero/química , Lecitinas , Disponibilidade Biológica , Anti-Hipertensivos , Administração Oral , Liberação Controlada de Fármacos , Polímeros/química , Portadores de Fármacos/química , Tamanho da Partícula
2.
Chemistry ; 29(72): e202302638, 2023 Dec 22.
Artigo em Inglês | MEDLINE | ID: mdl-37850687

RESUMO

In this letter, we designed a highly selective α-methylbenzylamine functionalized crown-ether-appended calix[4]arene derived phase transfer catalyst for asymmetric nitroaldol reaction to provide the desired nitroaldol adducts in high yields (up to 99 % yield) with good to excellent enantioselectivities (up to 99.8 % ee).

3.
J Org Chem ; 88(11): 7498-7503, 2023 Jun 02.
Artigo em Inglês | MEDLINE | ID: mdl-37218056

RESUMO

We report a class of quaternary ammonium Cinchona-functionalized crown ether-strapped calix[4]arene phase-transfer catalysts for the efficient enantioselective α-alkylation of glycine imines. The catalyst exhibits excellent catalytic performance at 0.1 mol % catalytic loading, affording the desired α-alkylated glycinates with 98% yield and 99.9% ee. The catalyst could be recovered and recycled up to 30 test cycles without a significant drop in activity.

4.
AAPS PharmSciTech ; 24(8): 213, 2023 Oct 17.
Artigo em Inglês | MEDLINE | ID: mdl-37848728

RESUMO

The anti-diabetic glipizide (GLN) drug has notable pharmaceutical advantages, but poor aqueous solubility restricts its wide applications. The present work was to develop a mixed polymeric micelle system composed of SA-F127 and TPGS to improve the water solubility and effective delivery of the GLN. First, we synthesized SA-F127 and confirmed it through FTIR, NMR, and GPC techniques. The GLN-PMM were fabricated with the thin-film technique and optimized with CCD design. The developed GLN-PMM was characterized using DLS, Zeta, TEM, Rheology, FTIR, DSC, and XRD measurements. The GLN-PMM manifested a spherical morphology with 67.86 nm particle size, a -3.85 mV zeta potential, and a 0.582±0.06 PDI value. The polymeric mixed micelles showed excellent compatibility with GLN and were amorphous in nature. NMR studies confirmed the encapsulation of GLN in the core of the mixed micelle. In addition, the GLN-PMM micelles were tested in vitro for cumulative drug release, ex vivo for permeation, and in vivo for anti-diabetic investigations. The GLN-PMM release profile in the various pH environments showed over 90% after 24 h, clearly indicating sustained release. The GLN-PMM micelles gave higher 88.86±3.39% GLN permeation from the goat intestine compared with free GLN. In-vivo anti-diabetic investigation proves the powerful anti-diabetic properties of GLN-PMM in comparison to the marketed formulation. These findings demonstrated that the polymeric mixed micelles of SA-F127 and TPGS could be a promising, effective, and environment-friendly approach for oral delivery of the GLN.


Assuntos
Sistemas de Liberação de Medicamentos , Micelas , Sistemas de Liberação de Medicamentos/métodos , Glipizida , Polímeros/química , Portadores de Fármacos/química , Tamanho da Partícula , Poloxâmero/química
5.
Inorg Chem ; 59(12): 8334-8344, 2020 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-32469208

RESUMO

Metal-organic frameworks derived nanostructures with extraordinary variability, and many unprecedented properties have recently emerged as promising catalytic materials to address the challenges in the field of modern organic synthesis. In this contribution, the present work reports the fabrication of an intricately designed magnetic MOF composite based on Mn-BDC (manganese benzene-1,4-dicarboxylate/manganese terephthalate) microflakes via a facile and benign in situ solvothermal approach. Structural information about the as-synthesized hybrid composite has been obtained with characterization techniques such as TEM, SEM, XRD, FT-IR, AAS, EDX, ED-XRF, and VSM analysis. Upon investigation of catalytic performance, the resulting material unveils remarkable efficacy toward facile access of a diverse array of pharmaceutically active 1,2,3-triazoles from a multicomponent coupling reaction of terminal alkynes, sodium azide, and alkyl or aryl halides as coupling partners. In addition to a wide substrate scope, the catalyst with highly accessible active sites also possesses a stable catalytic metal center along with superb magnetic properties that facilitate rapid and efficient separation. The prominent feature that makes this protocol highly desirable is the ambient and greener reaction conditions in comparison to literature precedents reported to date. Further, a plausible mechanistic pathway is also proposed to rationalize the impressive potential of the developed catalytic system in the concerned reaction. We envision that findings from our study would not only provide new insights into the judicious design of advanced MOF based architectures but also pave the way toward greening of industrial manufacturing processes to tackle critical environmental and economic issues.

6.
J Sci Food Agric ; 100(4): 1532-1540, 2020 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-31769023

RESUMO

BACKGROUND: Heavy metal resistant bacterium Enterobacter sp. C1D was evaluated for cadmium (Cd) mediated exopolysaccharide production, biofilm formation and legume root colonization ability under Cd stress to alleviate metal induced stress. RESULTS: The plant was sensitive to Cd (IC50 3-4 µg mL-1 ), whereas the bacterium showed high Cd tolerance (MIC99 120 µg mL-1 ). Confocal laser scanning microscopy of the Cajanus cajan roots showed heavy loads of green fluorescence protein labelled Enterobacter sp. C1D on the surface of plant root, specifically at the point of root hair/lateral root formation along with cortex, even under metal stress. The root colonizing ability of Enterobacter sp. C1D was not affected by the presence of Rhizobium and the bacteria could be observed after 30 days of incubation in soil. Various plant growth parameters, antioxidant metabolites and oxidative stress indicator were significantly influenced by bacterial treatment, which, overall, reduced the adverse effect of Cd. CONCLUSION: Heavy metal tolerant bacteria may be a good choice for the development of biofertilizers and may work well with the native soil microbes such as Rhizobium under the metal polluted soil. © 2019 Society of Chemical Industry.


Assuntos
Cádmio/metabolismo , Cajanus/microbiologia , Enterobacter/metabolismo , Raízes de Plantas/microbiologia , Cajanus/metabolismo , Enterobacter/crescimento & desenvolvimento , Estresse Oxidativo , Raízes de Plantas/metabolismo , Rhizobium/crescimento & desenvolvimento , Microbiologia do Solo , Poluentes do Solo/metabolismo
7.
Chirality ; 31(2): 91-96, 2019 02.
Artigo em Inglês | MEDLINE | ID: mdl-30565759

RESUMO

New efficient catalysts based on electrophilic N-fluoro quaternary ammonium salts are reported for catalytic allylation of (E)-N,1-diphenylmethanimine. The chiral version of the catalyst based on cinchonidine (F-CD-BF4 ) shows high catalytic activity with approximately 94% ee and TOF (>800 h-1 ). The F-CD-BF4 is prepared from cinchonidine and Selectfluor by one-step transfer fluorination.


Assuntos
Alcenos/química , Benzilaminas/química , Flúor/química , Nitrogênio/química , Catálise , Transporte de Elétrons , Modelos Moleculares , Conformação Molecular , Estereoisomerismo
8.
Environ Monit Assess ; 187(1): 4076, 2015 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-25384368

RESUMO

Persistence behavior of insecticides chlorpyriphos, profenofos, triazophos, cypermethrin, and deltamethrin following the use of three combination formulations Action 505 (chlorpyriphos + cypermethrin), Roket 44EC (profenofos + cypermethrin), and Anaconda Plus (triazophos + deltamethrin) was studied in cabbage following the spray application at the recommended and double doses. Bio-efficacy of these formulations was also evaluated against mustard aphids (Lipaphis erysimi Kaltenbach) and diamondback moth (Plutella xylostella L.). The residues of different insecticides persisted for 5-8 days at low dose and 8-12 days at high dose. The residues dissipated with time and 87-100% dissipation was recorded on the 8th day. The half-life values varied from 0.4 to 1.6 days. Based on the acceptable daily intake (ADI) values, a safe waiting period of 1 day has been suggested for the formulations Action 505 and Roket 44EC and 3 days for Anaconda Plus at the recommended dose of application. Action (1.6 L/ha) treatment was found to be the best as it significantly reduced the diamondback moth (DBM) (~60%) and aphid population (~70%) besides giving the highest yield (170% increase over control).


Assuntos
Brassica/química , Monitoramento Ambiental , Inseticidas/análise , Resíduos de Praguicidas/análise , Animais , Afídeos , Meia-Vida , Controle de Insetos/métodos , Inseticidas/toxicidade , Mariposas , Resíduos de Praguicidas/toxicidade
9.
Reprod Biol Endocrinol ; 12: 33, 2014 May 07.
Artigo em Inglês | MEDLINE | ID: mdl-24885775

RESUMO

BACKGROUND: A routine semen analysis is a first step in the laboratory evaluation of the infertile male. In addition, other tests such as measurement of reactive oxygen species can provide additional information regarding the etiology of male infertility. The objective of this study was to investigate the association of semen parameters with reactive oxygen species (ROS) in two groups: healthy donors of unproven and proven fertility and infertile men. In addition, we sought to establish an ROS cutoff value in seminal plasma at which a patient may be predicted to be infertile. METHODS: Seminal ejaculates from 318 infertile patients and 56 donors, including those with proven fertility were examined for semen parameters and ROS levels. Correlations were determined between traditional semen parameters and levels of ROS among the study participants. ROS levels were measured using chemiluminescence assay. Receiver operating characteristic curves were obtained to calculate a cutoff value for these tests. RESULTS: Proven Donors (n = 28) and Proven Donors within the past 2 years (n = 16) showed significantly better semen parameters than All Patients group (n = 318). Significantly lower ROS levels were seen in the two Proven Donor groups compared with All Patients. The cutoff value of ROS in Proven Donors was determined to be 91.9 RLU/s with a specificity of 68.8% and a sensitivity of 93.8%. CONCLUSIONS: Infertile men, irrespective of their clinical diagnoses, have reduced semen parameters and elevated ROS levels compared to proven fertile men who have established a pregnancy recently or in the past. Reactive oxygen species are negatively correlated with traditional semen parameters such as concentration, motility and morphology. Measuring ROS levels in the seminal ejaculates provides clinically-relevant information to clinicians.


Assuntos
Infertilidade Masculina/fisiopatologia , Estresse Oxidativo , Espécies Reativas de Oxigênio/metabolismo , Sêmen/metabolismo , Regulação para Cima , Centros Médicos Acadêmicos , Adulto , Biomarcadores/metabolismo , Fertilidade , Humanos , Infertilidade Masculina/diagnóstico , Infertilidade Masculina/metabolismo , Masculino , Ohio , Ambulatório Hospitalar , Estudos Prospectivos , Valores de Referência , Análise do Sêmen , Sensibilidade e Especificidade , Doadores de Tecidos
10.
Transpl Int ; 27(10): 1007-14, 2014 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-24852800

RESUMO

Deceased donor organ programme is still in infancy in India. Assessing deceased donation potential and identifying barriers to its utilization are required to meet needs of patients with organ failure. Over a 6-month period, we identified and followed all presumed brainstem dead patients secondary to brain damage. All patients requiring mechanical ventilation with no signs of respiratory activity and dilated, fixed and nonreacting pupils were presumed to be brainstem dead. All events from suspicion of brainstem death (BSD) to declaration of BSD, approach for organ donation, recovery and transplants were recorded. Subjects were classified as possible, potential and effective donors, and barriers to donation were identified at each step. We identified 80 presumed brainstem dead patients over the study period. The mean age of this population was 35.9 years, and 67.5% were males. When formally asked for consent for organ donation (n = 49), 41 patients' relatives refused. The conversion rate was only 8.2%. The number of possible, potential and effective donors per million population per year were 127, 115.7 and 9.5, respectively. The poor conversion rate of 8.2% suggests a huge potential for improvement. Family refusal in majority of cases reflects poor knowledge and thus warrants interventions at community level.


Assuntos
Morte Encefálica , Transplante de Órgãos/métodos , Doadores de Tecidos/provisão & distribuição , Obtenção de Tecidos e Órgãos/métodos , Adulto , Idoso , Estudos de Coortes , Seleção do Doador , Feminino , Hospitais Públicos , Humanos , Incidência , Índia , Unidades de Terapia Intensiva , Masculino , Pessoa de Meia-Idade , Transplante de Órgãos/estatística & dados numéricos , Estudos Retrospectivos , Medição de Risco , Adulto Jovem
11.
Chem Commun (Camb) ; 2024 Jul 23.
Artigo em Inglês | MEDLINE | ID: mdl-39041355

RESUMO

In this communication, we designed a highly selective camphor sulfonyl functionalized crown-ether-tethered calix[4]arene-derived organocatalyst for asymmetric Strecker reaction to provide the desired cyano adducts in high yields (∼99.9% yield) and enantioselectivities (up to 99.3% ee). Furthermore, 2 step facile syntheses of the antiplatelet drug (S)-clopidogrel exemplify the potential of this method for the preparation of commercial compounds.

12.
Assay Drug Dev Technol ; 22(2): 53-62, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38150562

RESUMO

This study aimed to develop a nanoparticle drug delivery system using poly (lactic-co-glycolic acid) (PLGA) for enhancing the therapeutic efficacy of lurasidone hydrochloride (LH) in treatment of schizophrenia through intramuscular injection. LH-loaded PLGA nanoparticles (LH-PNPs) were prepared using the nanoprecipitation technique and their physicochemical characteristics were assessed. Particle size (PS), zeta potential, morphology, % encapsulation efficiency, % drug loading, drug content, and solid-state properties were analyzed. Stability, in vitro release, and in vivo pharmacokinetic studies were conducted to evaluate the therapeutic efficacy of the developed LH-PNPs. The optimized batch of LH-PNPs exhibited a narrow and uniform PS distribution before and after lyophilization, with sizes of 112.7 ± 1.8 nm and 115.0 ± 1.3 nm, respectively, and a low polydispersity index. The PNPs showed high drug entrapment efficiency, drug loading, and drug content uniformity. Solid-state characterization indicated good stability and compatibility, with a nonamorphous state. The drug release profile demonstrated sustained release behavior. Intramuscular administration of LH-PNPs in rats resulted in a significantly prolonged mean residence time compared with the drug suspension. These findings highlight that intramuscular delivery of the LH-PNP formulation is a promising approach for enhancing the therapeutic efficacy of LH in treatment of schizophrenia.


Assuntos
Cloridrato de Lurasidona , Nanopartículas , Ratos , Animais , Copolímero de Ácido Poliláctico e Ácido Poliglicólico , Disponibilidade Biológica , Portadores de Fármacos/química , Ácido Poliglicólico/química , Ácido Poliglicólico/metabolismo , Ácido Láctico/química , Ácido Láctico/farmacocinética , Nanopartículas/química , Resultado do Tratamento
13.
Res Vet Sci ; 166: 105101, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38016218

RESUMO

This article aims to perform a comparative systematic review of regulations in veterinary medicine between the years 2016 to 2023. It explores the complex web of veterinary medicine regulations in various agencies and the nations, including USA (United States of America), EU (European Union), UK (United Kingdom), Japan, Australia, and India. Current article provides the comparative study on the veterinary regulations of different countries, including acts, directives, and drug approval processes. Such as, the specific legislation is needed to address zoonotic diseases. The strategic and regulated stockpiling of the veterinary drugs especially in chronic veterinary disease outbreak. It is essential to develop the dedicated Veterinary Pharmacopoeia for the regulated standardization of the raw materials as well as the formulations. Veterinary medical device is a field which is highly unregulated. There is a need to have regulations for the same. It is important to have dedicated veterinary pharmacovigilance centers which help in improving quality of medications to the livestock farms. After comparing the regulations of different countries. We observed that there is the absence of the zoonotic diseases and pharma stockpiling in every country. There is also an absence of the dedicated veterinary pharmacopoeia in every country. USA and Australia have the veterinary medical device regulation which is not there in other countries. Around the globe only Australia has the dedicated pharmacovigilance center. Including these recommendations into regulatory framework enhances the quality and safety of veterinary medicine. The current article adds a valuable resource for policymakers, veterinarians, and stakeholders in the field of animal health care.


Assuntos
Criação de Animais Domésticos , Médicos Veterinários , Animais , Humanos , União Europeia , Japão , Estados Unidos , Zoonoses
14.
Future Microbiol ; 18: 673-679, 2023 07.
Artigo em Inglês | MEDLINE | ID: mdl-37522244

RESUMO

Cruciferous vegetables and mustard oil are rich in the glucosinolate group of molecules. Isothiocyanates are an important group of glucosinolate derivatives. These derivatives have various bioactive properties, including antioxidant, antibacterial, anticarcinogenic, antifungal, antiparasitic, herbicidal and antimutagenic activity. Previous studies indicate that regular intake of such vegetables may considerably reduce the incidence of various types of cancer. These studies have inspired studies where the bioactive agents of these plants have been isolated and explored for their therapeutic applications. The use of these bioactive compounds as antifungals could be a new therapeutic approach against human pathogenic fungi. Isothiocyanates have been studied for their antifungal activity and have the potential to be used for antifungal therapy.


Vegetables like cabbage, cauliflower and broccoli have a distinct flavor because of chemicals called glucosinolates. Whenever we cut and eat these vegetables, glucosinolates are broken down into isothiocyanates. Glucosinolates and isothiocyanates have health benefits because they stop the growth of bacteria, parasites and fungi that cause disease, such as Candida albicans. They may also prevent cancer, as regularly eating these vegetables has been shown to reduce the development of some types of cancer in humans. Investigation is needed to explore how glucosinolates and isothiocyanates could be used to treat fungal infections.


Assuntos
Antifúngicos , Fungos , Isotiocianatos , Isotiocianatos/química , Isotiocianatos/farmacologia , Antifúngicos/química , Antifúngicos/farmacologia , Brassicaceae/química , Fungos/classificação , Fungos/efeitos dos fármacos , Fungos/metabolismo , Humanos , Micoses/dietoterapia , Micoses/tratamento farmacológico , Micoses/microbiologia , Verduras/química
15.
Nanoscale ; 15(34): 14007-14017, 2023 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-37539685

RESUMO

In this work, we fabricated a versatile and noble metal free copper-based heterogeneous photocatalyst, representing a green shift away from precious group metals such as Ir, Ru, Pt, which have been widely utilized as photocatalysts. The successfully synthesized and characterized copper photocatalyst was employed to establish a cross dehydrogenative coupling via C-H activation between tertiary amines and carbon nucleophiles. The highly efficient copper-based photocatalyst was characterized by numerous physico-chemical techniques, which confirmed its successful formation as well as its high activity. Inductively coupled plasma (ICP-OES) analysis revealed that the composite Cu@Xantphos@ASMNPs had a very high loading of 0.423 mmol g-1 of copper. The magnetic Cu@Xantphos@ASMNPs were utilized as a potential heterogeneous photocatalyst for the very facile and regioselective conversion of aryl tetrahydroqinoline to the respective nitroalkyl aryl tetrahydroisoquinoline in high yield using air as an oxidant and methanol as a green solvent with irradiation with visible light under mild reaction conditions. Additionally, the catalyst shows exceptional chemical stability and reusability without any agglomeration even after several cycles of use, which is one of the key features of this material, rendering it a potential candidate from economic and environmental perspectives.

16.
iScience ; 26(1): 105869, 2023 Jan 20.
Artigo em Inglês | MEDLINE | ID: mdl-36647377

RESUMO

Cubic spinel LiMn2O4 (LMO) are promising electrode materials for advanced technological devices owing to their rich electrochemical properties. Here, a series of Gd3+-doped LiMn2O4 were synthesized using a simple one-step sol-gel synthesis, and a systematized study on the effect of increasing Gd3+ concentration on magnetic properties is conferred. The Raman and density functional theory (DFT) calculations of the synthesized materials were correlated with the magnetic properties; we observed a high coercivity value for the doped LMO compared to pristine LMO, which scales down from 0.57T to 0.14T with an increase in Gd concentration. The samples exhibited paramagnetic (at 300K) to antiferromagnetic (at 5K) transition and variation in the magnetic moment due to the replacement of Mn+2 or Mn+3 ion by Gd+3 ion from the octahedral 16d lattice site. The observed phase transitions in the hysteresis curve below the Neel temperature (TN) at 5K are found to be due to the superexchange mechanism.

17.
Biomater Sci ; 11(15): 5136-5145, 2023 Jul 25.
Artigo em Inglês | MEDLINE | ID: mdl-37350291

RESUMO

In the present study, we sought to reveal how embedding oxidoreductase enzymes in a metal-organic framework influences restoring the biofunctionality when encapsulated within zeolitic imidazolate framework (ZIF-8 and ZIF-90), wherein these biocomposites were explored for their cellular metabolic activity using the (3-(4,5-dimethylthiazolyl-2)-2,5-diphenyltetrazolium bromide) (MTT) assay on A549 lung cancer cells and NIH3T3 (mouse fibroblasts) cells. We chose two biocomposites, namely catalase-encapsulated ZIF-8 and ZIF-90, wherein the enzyme was encapsulated at varied loadings through a rapid self-triggered nucleation around the protein surfaces of the enzyme. Interestingly, this embedding pattern of catalase in both ZIF-8 and ZIF-90 depended on the surface chemistry of the enzyme. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy analysis revealed the stability of the encapsulated enzyme in the nanospace of the ZIF-8 and ZIF-90 frameworks. Investigation of the cellular metabolic activity by the MTT assay of Cat@ZIF-8 and Cat@ZIF-90 on the lung cancer cell A549 showed cell viability enhancement in the case of Cat@ZIF-8 at a higher percentage compared to that of Cat@ZIF-90. A similar metabolic activity assay was performed with the internalization of Cat@ZIF-90 for NIH3T3 (mouse fibroblasts) cells. The revealed difference between the MOF compounds was due to the nano-confinement effect in ZIF-8 compared to ZIF-90, which can accelerate the utilization in cellar metabolic activity.


Assuntos
Exoesqueleto Energizado , Animais , Camundongos , Catalase , Células NIH 3T3
18.
Dalton Trans ; 52(32): 11303-11314, 2023 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-37530180

RESUMO

Two-dimensional (2D) graphene oxide nanosheets serve as an excellent support material for immobilizing metal complexes to deal with the drawbacks of homogeneous catalysis. In this work, we report a magnetically retrievable graphene oxide (MGO) based copper nanocatalytic system that has been efficiently exploited for obtaining a series of pharmaceutically and biologically active benzoxazole scaffolds. The nanocatalyst was designed by covalent immobilization of dehydroacetic acid (DHA) onto a magnetic amino-silanized graphene oxide nanosupport which was accompanied by its metallation with copper acetate. The structure of the synthesized MGO hybrid material (Cu@DHA@APTES@MGO) was characterized by numerous physico-chemical techniques such as transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometry (VSM), elemental mapping, atomic absorption spectroscopy (AAS), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET) surface area analysis and energy-dispersive X-ray fluorescence spectroscopy (ED-XRF). The fabricated architectures exhibited high efficiency for cyclization of 2-aminophenols and ß-diketones with wide substrate scope, excellent functional group tolerance, a higher conversion percentage (>98%) and a high turnover number (TON). The exceptional catalytic activity could be attributed to the 2D architecture of graphene oxide which provides space for trapping of reactants between 2D graphitic overlayers and metal surfaces and the reaction proceeds to afford benzoxazole products with moderate to excellent conversion percentages. Notably, this nanocomposite could be recovered easily through an external magnetic force and reused for multiple runs without any appreciable loss in its catalytic efficacy.

19.
Nanoscale ; 15(7): 3482-3495, 2023 Feb 16.
Artigo em Inglês | MEDLINE | ID: mdl-36723031

RESUMO

The intriguing features of surface-engineered hexagonal two-dimensional boron nitride (h-BN) nanostructures have captivated the immense interest of researchers working in the arena of materials science. Inspired by striking attributes exhibited by h-BN nanosheets as the support material, we devoted our efforts towards synthesizing a novel magnetically retrievable h-BN/Fe3O4/APTES-AMF/CuII catalytic system, which was then comprehensively characterized using various techniques including SEM, TEM, EDX, SEM-based elemental mapping, ED-XRF, AAS, XRD, FT-IR, VSM, XPS, TGA, and BET. Further, the catalytic potential of h-BN/Fe3O4/APTES-AMF/CuII nanocomposites was investigated in the one-pot multicomponent coupling reaction to gain access to a library of biologically active 2-amino-4-aryl(or heteroaryl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitriles under ambient conditions. In addition, the use of green solvent, facile magnetic recoverability, and reusability of up to six successive runs made this protocol environmentally benign and economical. This work throws light on the development of covalently functionalized 2D-BN nanostructure-based copper catalysts and establishes its significance in furnishing industrially demanding products that would pave the way towards sustainable chemistry.

20.
Dalton Trans ; 53(1): 82-92, 2023 Dec 19.
Artigo em Inglês | MEDLINE | ID: mdl-38037690

RESUMO

Lithium-sulfur (Li-S) batteries have attracted much attention due to their superior theoretical specific capacity and high theoretical energy density. However, rapid capacity fading originating from the shuttle effect, insulating the S cathode and the dendrite formation on the Li anode restrict the practical applications of Li-S batteries. Herein, we suggest novel coatings on glass fiber separators to satisfy all high-performance Li-S battery requirements. A conductive Ti3C2Tx (MXene) nanosheet/Fe-MOF or Ti3C2Tx (MXene) nanosheet/Cu-MOF layer was coated on a glass fiber separator to act as a polysulfide trapping layer. The MXene layer with high conductivity and polar surface functional groups could confine polysulfides and accelerate the redox conversions. The porous MOF layer acts as a Li ion sieve, thereby leading to the interception of polysulfides and mitigation of Li dendrite growth. The cells with the Cu-MOF/MXenes and Fe-MOF/MXene separators display superior capacities of 1100 and 1131 mA h g-1 after 300 cycles, respectively, whereas the cell with a pure glass fiber separator delivers a very low capacity of 309 mA h g-1 after 300 cycles. With Fe-MOF/MXene and Cu-MOF/MXene configurations, the discharge capacity, coulombic efficiency, cycling stability, and electrochemical conversion reactions are significantly improved. Our ab initio calculations demonstrate that the MXene layer dissociates lithium polysulfides into adsorbed S and mobile Li ions, which explains the experimental findings.

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