Pot Synthesis Research Articles

One Pot Synthesis of New Benzimidazole Derivatives with Exceptionally High Luminescence Quantum Efficiency.

There are different approaches to the synthesis of benzimidazole. In this article, five new benzimidazole derivatives, BMPO, Me-BMPO, Di-MeBMPO, F-BMPO and Cl-BMPO where (BMPO=3-[(1H)-benzo[d]imidazol-2-yl]pyridin-2(1H)-one), have been prepared. Another study was carried out on luminescence properties and their potential applications for the detection of transition metal ions. From the one-pot synthesis approach, all the derivatives of the benzimidazole compounds were obtained. The compounds were characterized using HRMS, 1HNMR, 13CNMR, and X-ray crystallography. Herein, a mechanism has been deciphered by predicting the release of HCl(g). All compounds showed a strong deep blue emission when dissolved in dimethylacetamide (DMA), with emission wavelengths at 423, 428, 435, 423, and 421 nm, and half-times of 3.64, 2.77, 2, 19, 3.42 and 3.52 ns, respectively. In addition, their emission quantum yields were determined to be 72, 50, 42, 73 and 80%. Five new benzimidazole derivatives, BMPO, Me-BMPO, Di-MeBIPO, F-BIPO, and Cl-BIPO, have been successfully synthesized by the one-pot synthesis method, and their structures are characterized and confirmed. The compounds exhibited exceptional luminescence by emitting a strong blue light in DMA with high fluorescence quantum yields between 42~80%.

One pot synthesis of donor-acceptor carbon nitride with distinct thiophene rings accelerate photocatalytic hydrogen evolution

Graphitic carbon nitride (g-CN) with a donor-acceptor structure was synthesized by urea and cross-linking thiophene precursors at the terminal sites, achieved through calcination of urea with four different thiophene-based precursors under atmospheric conditions. Among these, UDB-2-1, which incorporates dibenzothiophene-2-carboxyaldehyde (DB-2) 1 mg, demonstrated a hydrogen evolution activity of 650 μmol/g·h, approximately six times higher than pristine graphitic carbon nitride (U). The apparent quantum yield (AQY) was measured to be 4.01 %, 4.89 %, and 3.72 % at 400 nm, 420 nm, and 450 nm, respectively, in the presence of potassium hydrogen phosphate (KPH). This enhanced performance is attributed to increased visible light absorption from the n-π∗ transition introduced by the thiophene ring and enhanced charge separation due to the donor-acceptor (DA) structure, with DB-2 acting as an electron donor. Prepared photocatalysts were characterized by XRD, XPS, FTIR, SEM, TEM, BET, ESR, EIS, Mott-Schottky, DRS, PL, and TRPL measurement. This study provides a simple and effective strategy to improve carbon nitride performance and underscores the importance of functional group positioning and structural isomers in molecular design for solar-energy applications.

One Pot Synthesis of New Powerful Building Blocks in 1,8-Naphthalimide Chemistry

This communication reports a reliable one-pot synthetic protocol for preparation on a multigram scale of 3-bromo- and 3,4-dibromo-6-nitro-1,8-naphthalic anhydride from commercially available and economical 1,8-naphthalic anhydride. The synthetic steps used were nitration and selective bromination in sulfuric acid at room temperature. The reaction takes place under mild conditions and is completely controllable depending on the equivalents of the brominating reagent used. Both anhydrides are powerful building blocks in naphthalimide chemistry. In addition, their imides and esters were also synthesized.

Preparation of Ni/Bentonite Acid-Activated using Dragon Fruit Peel Extract (Hylocereus polyrhizus) As a Reductor for One Pot Synthesis of Menthol

Ni/Bentonite is acid-activated has been synthesized using dragon fruit peel extract (Hylocereus polyrhizus) as a reductor through an impregnation method. This research aims to characterize Ni/Bentonite acid-activated using dragon fruit peel extract as a reductor based on FTIR and XRD instruments and to analyze the product obtained in one pot synthesis of menthol from citronellal using Ni/Bentonite acid-activated catalyst. Preparation of Ni/Bentonite acid-activated catalyst was carried out using a wet impregnation method with dragon fruit peel extract as a natural reductor. The successful synthesis of Ni/Bentonite acid-activated was confirmed by FTIR spectrum identification, showing absorptions at wavelengths of 1049.28 cm?¹ and 694.37 cm?¹, indicating Si-O groups in the bentonite, and XRD diffractogram indicating the presence of Ni at diffraction peaks of 2? = 40.5° and 2? = 47.74°. The catalyst was able to convert menthol by 0.77% through one pot synthesis without using H? sources such as potassium formate.

Multicomponent one pot synthesis of substituted pyridines with a highly active and recyclable hydrotalcite-lanthanum nanocatalyst

Herein, the synthesis of 2-amino-3,5-dicyano-6-sulfanyl pyridine derivatives has been studied due to wide applications of highly substituted pyridines. At first, Hydrotalcite (HT) with various loading amounts of lanthanum (HT-La) was synthesized. Then, their catalytic activities were investigated for the condensation reaction of benzaldehyde, malononitrile, and thiophenol under reflux condition as a model reaction. The prepared HT nanocatalyst with 10 mol% of La showed the best performance in this multicomponent reaction. In addition, the reusability of the nanocatalyst was studied and the results showed, that the prepared nanocatalyst could be reused several times with an only moderate decrease in activity. Subsequently, HT-La (10 mol%) efficiently catalyzed the one-pot condensation reaction for the synthesis of highly substituted pyridines under reflux conditions. The products were produced with excellent yields, short reaction times, and easy recyclability of the nanocatalyst.

Antimicrobial Effect of Waterborne Polyurethane-Based Cellulose Nanofibril/Silver Nanoparticles Composites and Acacia concinna (Willd.) DC Extract (Shikakai).

Antimicrobial coatings are becoming increasingly popular in functional material modification and are essential in addressing microbial infection challenges. In this study, the phytochemical and antimicrobial potential of aqueous, 80% methanol and 80% ethanol pod extracts of Acacia concinna (Willd.) DC (AC) and its application in the green in situ (one pot) synthesis of silver nanoparticles on Cellulose nano fibrils (CNF) and Waterborne polyurethane (WPU) were prepared. The phytochemical evaluation of Acacia concinna crude extracts showed the presence of alkaloids, flavonoids, phenols, tannins, terpenoids, saponins, steroids. The surface plasmon Resonance peak of CNF/AC-AgNPs was 450 nm and the FTIR result confirmed functional groups such as carbonyl, phenols and carboxyl were present which was important for the bio-reduction of silver nanoparticles. The crude AC aqueous pods extract against Gram-positive and Gram-negative bacteria compared with AC ethanol and AC methanol extracts. The WPU/CNF/AC-AgNPs composite dispersion was also good in terms of its antibacterial activities. The WPU/CNF/AC-AgNPs nanocomposites could be applied as bifunctional nanofillers as an antimicrobial agent in food packaging systems and other biological applications.

One Pot Synthesis of Thiopyrimidine Derivatives from Lignin Reproductions by Microwave-Assisted Ultrasonic Microscopy with DFT Description for Clarifying the Mass Spectrum

In this work, an efficient and sustainable procedure for the one-pot synthesis of thiopyrimidine derivatives starting 1,3-diketone cut off β-O-4 lignin precursors to create anticancer agents. Microwave-ultrasonic assisted lignin extract in accessing various heterocyclic precursors such as pyrimidine, pyridine, and thiophene moieties. The results designated the ultrasonic-assisted microwave significantly accelerated synthesis with reduced time. We have diversely prolonged to tight-binding approaches to the electron ionization mass spectrometry with quantum stimulation (DFT/EIMS) to examine electron ionization mass spectra correlated to the experiment. Moreover, DFT/EIMS provides into the mechanism of the reaction of mass spectra trials. It cabins on the fragmentation method to raise the challenging bond breaking and structural rearrangements. The quantum chemical process for effective precursors of a mass spectrum is exactness required and discussed. Foremost fragmentation designs are studied and related to experimental data of the pyrimidin-thione derivatives and their glycosides.

Anion-intercalation pseudocapacitance in oxygen vacancy-rich spinel-perovskite NiFe2O4-LaFeO3 nanocomposite for high energy density asymmetric supercapacitor application

Oxide nanomaterials have attracted significant attention as energy storage materials. The combination of spinel-perovskite oxides as nanocomposites creates dense oxygen vacancies (VO) at the hetero-interface. VO present in the complex oxides are indispensable for energy conversion applications. Herein, we demonstrated the one pot synthesis of spinel-perovskite NiFe2O4-xLaFeO3 nanocomposite and investigated the phase formation using variable temperature powder X-ray diffraction of the gel precursor. The role of oxygen-vacancy mediated tuneable redox transitions in NiFe2O4-xLaFeO3 nanocomposite has been understood. The anion-intercalation-based pseudocapacitance and the oxygen intercalation have been exploited for high-performance electrochemical energy storage. The NiFe2O4–2LaFeO3 exhibited a high specific capacity of 652 C g−1 at a current density of 2 A g−1. The fabricated NiFe2O4–2LaFeO3||NiCo2O4 asymmetric supercapacitor device (ASC) exhibited excellent cyclability over 20,000 cycles with superior capacity retention and high Coulombic efficiency (92 %) and achieved a high energy density of 42.5 Wh kg−1 at a power density of 1500 W kg−1. The presence of VO and the mixed-valence states of Fe2+/3+ were confirmed by XPS-depth profiling. The tuneable redox transition of Fe2+/3+ and VO contribute to the higher pseudocapacitance response.

One Pot Synthesis of Alkyl Nitriles

A one-pot synthesis method to produce alkyl nitriles using the corresponding aliphatic carboxylic acid has been developed. The process involves treating the aliphatic acid with thionyl chloride to obtain the corresponding aliphatic acid chloride, which is then further treated with anhydrous ammonia gas to yield the respective aliphatic acid amide. The intermediate corresponding amide is dehydrated with thionyl chloride to obtain alkyl nitrile with a quantitative yield.

An Efficient One Pot Synthesis and Biological Activities of 6H-Indolo[2,3-b]quinoxalines Promoted by Palladium Acetate as Catalyst

An Efficient One Pot Synthesis and Biological Activities of 6H-Indolo[2,3-b]quinoxalines Promoted by Palladium Acetate as Catalyst

Facile One Pot Synthesis of Hybrid Core-Shell Silica-Based Sensors for Live Imaging of Dissolved Oxygen and Hypoxia Mapping in 3D Cell Models.

Fluorescence imaging allows for noninvasively visualizing and measuring key physiological parameters like pH and dissolved oxygen. In our work, we created two ratiometric fluorescent microsensors designed for accurately tracking dissolved oxygen levels in 3D cell cultures. We developed a simple and cost-effective method to produce hybrid core-shell silica microparticles that are biocompatible and versatile. These sensors incorporate oxygen-sensitive probes (Ru(dpp) or PtOEP) and reference dyes (RBITC or A647 NHS-Ester). SEM analysis confirmed the efficient loading and distribution of the sensing dye on the outer shell. Fluorimetric and CLSM tests demonstrated the sensors' reversibility and high sensitivity to oxygen, even when integrated into 3D scaffolds. Aging and bleaching experiments validated the stability of our hybrid core-shell silica microsensors for 3D monitoring. The Ru(dpp)-RBITC microparticles showed the most promising performance, especially in a pancreatic cancer model using alginate microgels. By employing computational segmentation, we generated 3D oxygen maps during live cell imaging, revealing oxygen gradients in the extracellular matrix and indicating a significant decrease in oxygen level characteristics of solid tumors. Notably, after 12 h, the oxygen concentration dropped to a hypoxic level of PO2 2.7 ± 0.1%.

One pot synthesis and crystal of N-benzoyl(benzo)thiazol-2-amine borodifluoride complexes (NBO) with aggregation induced luminescence properties

In this paper, N-benzoyl(benzo)thiazol-2-amine borodifluoride complexes (NBOs) were synthesized directly from benzoyl chloride and (benzo)thiazol-2-amine by one-pot method. The molecular structures of the target compounds were characterized by nuclear magnetic resonance (NMR), high resolution mass spectrometry and single crystal X-ray diffraction. The optical properties of the compounds were measured by UV–Vis absorption and fluorescence spectra. In CH2Cl2, this compounds exhibit large Stokes shifts, the maximum absorption peaks of NBO-1, NBO-2 and NBO-3 are 327 nm, 342 nm and 362 nm, and the maximum emission peaks are 400 nm, 442 nm and 498 nm, respectively. It can also be found that the absorption and emission spectra are redshifted with the increase of the conjugated system. Further more, we found that NBO-2 and NBO-3 molecules with additional benzo structure have the properties of aggregation induced emission, while NBO-1 show weak fluorescence in both solution and aggregation state.

One pot synthesis of 4-iodo-3-phenylbenzo[b][1,6]naphthyridine via imino iodization-cyclization of alkynylquinoline-3-carbaldehydes

Simple, environmentally benign and metal free one pot strategy has been used for the synthesis of 4-iodo-3-phenylbenzo[b][1,6]naphthyridine from O-alkynylquinolinyl aldehydes with tert-butyl amine and iodine through imine formation in good to excellent yield at room temperature in aerobic and mild conditions. The beauty of this reaction is the imine formation and cyclization in the same reaction pot. Due to presence of iodine in product, it can be useful for further reaction and can be valuable synthon for new organic compounds.

Solid Solution Behavior of High Performance BiOBrxI1-X Photoanodes Probed Using Solid-State NMR, XRD and Optical Spectroscopy

Bismuth oxyhalides (BIOX) are a family of solution-synthesizable 2D layered semiconductors constituted of earth-abundant elements namely bismuth, oxygen and the halogens. BIOX based thin films and heterojunctions are the subject of immense scientific interest due to their impressive performance in photocatalytic and photoelectrochemical devices. Solid solutions of Br/I bismuth oxyhalides exhibit continuously tunable absorption and emission spectra similar to that observed in mixed halide MAPbClxBryI3-x-y perovskites and mixed anion III-V GaAsxP1-x semiconductors. The excited state decay showed two components for all the mixed halide BiOX semiconductors with a dominant short-lived component in the nanosecond range and a weaker longer-lived component of ~100 ns. The average photoluminescence (PL) lifetime varied from 5.4 ns in bare BiOI to 1.49 ns in bare BiOBr with intermediate compositions exhibiting monotonically increasing average PL lifetimes with increasing iodine content. Using a combination of characterization techniques such as solid-state nuclear magnetic resonance (ssNMR), x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS) and optical spectroscopy, we demonstrate the formation of atomic level solid solutions in Br/I bismuth oxyhalides. Through refinement of the lattice parameters using powder XRD and complementary atomic-level 209Bi SSNMR spectroscopy, we found that Vegard's law was obeyed by the BIOBrxI1-x solid solutions. By varying the Br:I ratio, it is also possible to tune the electronic band gap as well as the energy levels corresponding to the conduction band minimum (ECB, min) and the valence band maximum (EVB, max), thus allowing control over the thermodynamic driving force available to drive chemical reactions using photogenerated or electrically injected charge carriers. Suppression of the longitudinal optical phonon in solid solutions of Br/I bismuth oxyhalides is suggestive of lower phonon scattering of charge carriers and improved electronic transport. A synergistic enhancement of more than 1 order of magnitude in the photoelectrochemical water-splitting performance was obtained for the optimized solid solution (BiOBr0.67I0.33) under AM 1.5G 1 sun illumination. Our results pave the way for a one pot synthesis protocol to form BiOX thin films, powders and colloidal suspensions with deterministic control over the stoichiometry.

One Pot Synthesis of Phosphomolybdenate Based Hybrids for Efficient Oxidative Desulfurization

With increasing stringent standard of sulfur content in fuels, there is a growing need for high-efficiency deep desulfurization to meet ecological and environmental demands. Herein, a series of heteropolyacid catalysts with phosphomolybdic acid base melamine (MHPMo-n) were synthesized by one-pot method and applied to oxidative desulfurization. Further, the optimum conditions for desulfurizations could be explored, which the desulfurization rate of the catalyst could reach 100% within 60 min under the conditions of m(catalyst)= 0.01 g, T = 40 °C, O/S = 3. Furthermore, the catalyst demonstrated excellent catalytic efficiency during the five cycles. One-pot method of phosphomolybdic acid base melamine provides a new idea for the synthesis of catalysts with outstanding catalytic properties for oxidative desulfurization (ODS).

Synthesis and Characterization of Metal Complexes [M(L)(Im)]NO3, In Vitro DNA/BSA Binding Behavior and Cytotoxicity on HepG2 Cancer Cells

AbstractA new ligand (HL) was prepared from heterocyclic 8‐Hydroxy‐2‐quinolinecarboxaldehyde and 2‐Aminobenzophenone in one pot synthesis. The metal complexes of the types [Zn(L)(Im)]NO3 (1), [Cu(L)(Im)]NO3 (2) and [Co(L)(Im)]NO3 (3) were prepared by adopting HL and Imidazole under refluxing conditions. The HL and complexes 1–3, were characterized by CHN elemental analysis and spectroscopic methods 1H NMR, 13C NMR, FT‐IR, ToF Mass. The spectroscopic studies suggest square pyramidal geometry in all complexes. The interaction of ligand and complexes with DNA and BSA was conducted by UV‐vis absorption and fluorescence spectroscopy. The Kb value of 2.17×104 M−1 for complex 2 is the highest depicting its greater binding propensity with DNA. Similarly, in BSA binding studies, complex 2 shows greater binding potential in the hydrophobic core probably near the Trp 212 in the subdomain IIA. Furthermore, the complex 2 shows excellent cytotoxicity on HepG2 cancer cells with IC50=74.05±0.69 μM. In the cell cycle analysis of HepG2 cells, it has been observed that complex 2 arrests the cell proliferation in the G1/S phase. Annexin V‐based flow cytometry analysis further indicated 6‐fold apoptotic cell death by complex 2 in the experiment along with non‐specific necrosis cell death.

One pot synthesis of novel C3N4/C nanosheet composites under environmental benign molten salts for peroxymonosulfate activation with enhanced efficiency and reusability

The application of g-C3N4 based carbon materials in peroxymonosulfate (PMS) activation has faced challenges due to the electrochemically inert nature of nitrogen without light irradiation. In this study, two types of crystalline C3N4/C nanosheet composite catalysts were synthesized from glucose and dicyandiamide (DCD) via molten salt-assisted pyrolysis, denoted as M-GD and M-GD2. Both the composite catalysts showed significant improvement in the degradation of acid orange 7 amid PMS activation, taking the advantages of high graphitic N content and defect degree. Specifically, M-GD2 with excessive dosage of DCD exhibited a record catalyst specific activity value (0.0925 L min−1 m−2) in comparison with conventional C3N4 based carbon catalysts. The study also examined the effects of catalyst and PMS concentrations, temperatures, initial pH, and impurity ions on catalytic activity, as well as the catalytic performance in actual sludge wastewater cases. Notably, the M-GD2 catalyst exhibited exceptional regeneration capacity after four consecutive tests, attributed to its unique 3D structure comprising g-C3N4 nanoparticles loaded on crystalline C3N4/C nanosheets. Mechanism analysis revealed that a non-radical mechanism predominantly drove the PMS activation reaction, primarily involving catalyst-mediated electron transfer and surface-bound radicals due to the formation of catalyst-PMS* complexes. This work presents a facile and economical method for preparing defect-rich crystalline C3N4/C nanosheet composite with high graphitic N content, highlighting its catalytic activity, reusability, and regeneration performance synchronously. These findings contribute to advancing the field of PMS activation and offer promising applications in water environment remediation.

Harnessing synergies: Gold-polyaniline based symmetric supercapacitor for low-frequency waveform generation

Electrochemical supercapacitors, one of the storage devices, have attracted much attention owing to their high power density, fast charge-discharge and long cycle life. In this study, we present findings of a hybrid system comprised of gold and polyaniline, fabricated via an in-situ, one pot synthesis route and designed for use in symmetric supercapacitor applications. The gold-polyaniline (Au-PANI) based hybrid material was thoroughly characterized using microscopic, optical, and surface analytical techniques to gain a comprehensive understanding of the system. The electrochemical performance of Au-PANI based electrode was examined using cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) techniques. The hybrid system exhibited maximum specific capacitance (CS) 387 F/g at the current density of 12 A/g for three electrode system. The symmetric supercapacitor exhibited a maximum specific capacity (QS) 303 mAh/g at the current density of 0.1 A/g and achieved a maximum energy density (ED) and power density (PD) of 243 mWh/kg and 619 W/kg at the current density of 0.1 A/g and 0.9 A/g, respectively. Further, the Au-PANI based symmetric device was applied to generate low-frequency waveforms.

Microwave assisted facile one pot synthesis of novel pyrazole derivative for multi-analyte detection (Fe3+ and Zn2+) and its solvatochromic studies

A novel heterocyclic pyrazole-based probe Ph-DB was synthesised by microwave assisted concatenation of phenyl hydrazine and 2,5-dibromo-3-thiophenecarboxylaldehyde. The veracity of synthesized pyrazole derivative was established using 1H NMR,13C NMR, HRMS and FT-IR. ICT studies were conducted in different organic solvents of varying polarity to comprehend the solvatochromic nature of compound. DFT studies were performed to elucidate the intricacies of the Ph-DB’s electronic structure. The electrochemical band gap and optical band gap were calculated using cyclic voltammetry and Tauc's plot respectively. SEM analysis was carried out to explore the surface morphology of Ph-DB which was found to show small microwires like structures which supports optoelectrical properties of Ph-DB. The photophysical studies were carried out to check the chromogenic and fluorogenic response of Ph-DB towards different metal ions. It was observed that Ph-DB shows noticeable fluorescence enhancement with Zn2+ ions with the detection limit of 6.1 µM and chromogenic change with Fe3+ with a detection limit of 6.6 µM. Additionally quantum yield, binding constant and recovery experiment of Ph-DB probe were performed. Ph-DB probe was utilised for precise monitoring of Zn2+ and Fe3+ ions in water samples.

Talc: A natural mineral base catalyst for the one pot synthesis of bis(pyrazolyl)methane derivatives under thermal and solvent-free conditions

In this work, we were decontaminated the ore to extract the talc, directly. Then, we used talc as a heterogeneous basic catalyst for one pot synthesis of bis(pyrazolyl)methane derivatives via the condensation of ethylacetoacetate, hydrazine hydrate and aromatic aldehyde derivatives under thermal and solvent-free conditions. This solid type of catalyst was identified by fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), energy-dispersive X-ray spectroscopy (EDS), EDS mapping and Brunauer–Emmett–Teller (BET) theory. Heterogeneous and solvent-free conditions, catalyst recyclability, high yields of the products and short reaction times are some advantages of this method. The reusability of the catalyst was examined for five times and it was successfully used in each run without any significant decreasing in its activity.