Synthetic routes of chromene are an area of thrust research due to its wide application as pigments, agrochemicals, cosmetics, and an important nucleus scaffold for various pharmaco-logically active drugs. The chromene nucleus is an important moiety for the discovery of new drug candidates owing to its broad range of pharmacological actions like antitumor, anti-inflammatory, antiviral, and many others. However, traditional synthesis techniques frequently use unsafe reagents and produce hazardous waste, presenting environmental issues. The eco-friendly production of chromene derivatives utilizes sustainable raw materials, non-toxic cata-lysts, and gentle reaction conditions to reduce ecological consequences. Innovative methods like microwave irradiation, ultrasound synthesis, the use of environmentally friendly solvents, a cata-lyst-based approach with minimal environmental impact, and mechanochemistry-mediated syn-thesis are implemented. These approaches provide benefits in scalability, cost-effectiveness, and ease of purification. This review compiles and presents various recently reported green synthetic strategies of chromene and its derivatives and gives the reader a clear idea of the detailed and crit-ical aspects of various synthetic protocols described.

This work uses green sustainable reactions twice. Firstly, it is microwave synthesis: 2,4,6-tribiphenyl-4-yl-1,3,5-triazine and similar compounds were prepared in a closed microwave reactor in n-octane by the Friedel-Crafts reaction. Second, a hybrid electrocatalyst for the highly demanded electrochemical reaction of nitrate reduction to ammonia (NO3RR) was prepared based on this material. This reaction has great potential to replace the energy-intensive Haber-Bosch process, and in addition, has independent value for the elimination of nitrate contamination of water resources. As shown in the work, microwave synthesis is an eco-friendly method for the synthesis of complex organic compounds; fast, selective and with a high yield of the target product. The electrocatalyst deposited on the graphite electrode consisted of a layer of 2,4,6-tribiphenyl-4-yl-1,3,5-triazine and related compounds coated with cobalt oxide. The hybrid catalyst was firmly retained on the graphite electrode during NO3RR and the material showed impressive stability with almost no decrease in catalytic activity even after the fifth cycle. Both 2,4,6-tribiphenyl-4-yl-1,3,5-triazine and the catalyst based on this substance were characterized by SEM, XPS, XRD, UV-vis spectra, cyclic (and linear) voltammetry, and chronoamperometry. This work can serve as a starting point for the development of stable and durable electrocatalysts for NO3RR using triazine derivatives.

Controlled drug delivery systems offer numerous advantages. This research evaluates Opuntia leaf mucilage grafted with polyacrylamide (OPM-g-PAM) as a promising controlled-release polymer. PAM chains were grafted onto the backbone of OPM using a microwave-assisted method. Optimization of the best grade was based on % grafting efficiency and intrinsic viscosity, followed by extensive physical and analytical characterizations. Analytical characterizations revealed semicrystalline nature of the biomaterial. SEM and AFM observations revealed rough and porous surfaces, indicating effective grafting. Swelling behavior showed maximum sensitivity at pH 7, with reduced swelling at higher sodium chloride concentrations. A comparative study of % drug release of Rosuvastatin over 24 h showed that the optimized grade controlled drug release effectively, achieving 78.5 % release compared to 98.8 % for GF-3. The release data fitted the Korsmeyer-Peppas model, with an \"n\" value of 0.8334, indicating non-Fickian (anomalous) diffusion. Bacterial biodegradability studies confirmed the high biodegradability of the graft copolymer. In vitro acute toxicity tests showed no toxicity, as confirmed by histopathological studies of heart, liver, and kidney. Overall, the results indicate that OPM-g-PAM is a highly promising material for use in drug delivery systems, demonstrating potential as a novel controlled-release polymer.

In this work, the selenylation Codonopsis pilosula polysaccharide (Se-CPPS) were synthesized using an optimized microwave-assisted method. Then, physicochemical properties, including molecular weight, particle size, valence state of selenium, antioxidant capacity, release mechanism of selenium under gastrointestinal conditions, as well as their effects on HT-29 cell viability were comprehensively investigated. The results demonstrated that Se-CPPS with the highest selenium content (21.71 mg/g) was synthesized using 0.8% nitric acid concentration under microwave conditions of 90 min at 70 °C. FTIR and XPS analysis revealed that Se was bound to the polysaccharide chain in the form of O-Se-O and O-H···Se, with a valence state of either 0 or +4. In vitro investigations on antioxidant activity and selenium release capacity indicated that selenization not only enhanced the antioxidant activity of CPPS but also endowed Se-CPPS with robust selenium release capability in simulated gastric digestion. The effects of Se-CPPS on HT-29 cells was further investigated by CCK-8 method. The results showed that the selenide modification effectively reduced the toxicity of Na2SeO3 and enhanced the viability of CPPS. The findings of this study offer valuable methodological guidance for the synthesis of Se-polysaccharides with superior functional properties.

The study aimed to understand how changes in crystal\'s size affect the lattice parameters and crystal structure of Mg1-xNixO solid solution for six X values ranging from x = 0 to x = 1. Mg1-xNixO was synthesized via two different wet-chemical techniques: the sol-gel and the microwave hydrothermal method, both followed by calcination at different temperatures of 673, 873, 1073, 1273 and 1473 K. As annealing caused grain growth, the varied temperature range allowed to examine a wide range of grain sizes. The lattice parameters and x values were determined from XRD (X-ray diffraction) peak positions and intensities respectively. The grain size was evaluated by XRD line profile analysis and supported by SEM (scanning electron microscope) observations. At the temperatures of 673 and 873 K grain size was in the nanometric range and from 1073 K and above grain size was in the micrometric range. A non-monotonic lattice variation versus grain size was found for each concentration. When grain size decreased there was a slight contraction, however for grain size in the nanometric range there was a severe lattice expansion. Both lattice parameter changes were explained by two effects acting together: contraction due to surface stress and expansion due to weakening of the ionic bonding at nanocrystalline particles. In this current research study, the lattice parameter was mapped in two dimensions: concentration and grain size. The findings of this study provided valuable insights into the lattice variation in the MgO-NiO solid solution system.

The synthesis of covalent organic frameworks (COFs) at bulk scale require robust, straightforward, and cost-effective techniques. However, the traditional solvothermal synthetic methods of COFs suffer low scalability as well as requirement of sensitive reaction environment and multiday reaction time (2-10 days) which greatly restricts their practical application. Here, we report microwave assisted rapid and optimized synthesis of a donor-acceptor (D-A) based highly crystalline COF, TzPm-COF in second (10 sec) to minute (10 min) time scale. With increasing the reaction time from seconds to minutes crystallinity, porosity and morphological changes are observed for TzPm-COF. Owing to visible range light absorption, suitable band alignment, and low exciton binding energy (Eb=64.6 meV), TzPm-COF can efficaciously produce superoxide radical anion (O2 .-) after activating molecular oxygen (O2) which eventually drives aerobic photooxidative amidation reaction with high recyclability. This photocatalytic approach works well with a variety of substituted aromatic aldehydes having electron-withdrawing or donating groups and cyclic, acyclic, primary or secondary amines with moderate to high yield. Furthermore, catalytic mechanism was established by monitoring the real-time reaction progress through in situ diffuse reflectance infrared Fourier transform spectroscopic (DRIFTS) study.

The sustainable microwave (MW) synthesis of hydroxyapatite (HAp) from decarbonized eggshells was investigated. Decarbonization of eggshells, as a natural source of calcium carbonate (CaCO3), was carried out in the current study at ambient conditions to reduce the footprint of CO2 emissions on our environment where either calcination or acidic direct treatments of eggshells produce CO2 emissions, which is a major cause for global warming. Eggshell decarbonization was carried out via the chemical reaction with sodium hydroxide (NaOH) alkaline solution in order to convert eggshell waste into calcium hydroxide (Ca(OH)2) and simultaneously store CO2 as a sodium carbonate (Na2CO3) by-product which is an essential material in many industrial sectors. The produced Ca(OH)2 was mixed with ammonium dihydrogen phosphate (NH4H2PO4) reagent at pH~11 before being subjected to MW irradiation at 2.45 GHz frequency for 5 min using 800 Watts to prepare HAp. The prepared Nano-HAp was characterized using X-ray diffraction (XRD) where the crystal size was ~28 nm using the Scherrer equation. The elongated rod-like nano-HAp crystals were characterized using scanning electron microscopy (SEM) equipped with dispersive energy X-ray spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM). MW synthesis of decarbonized eggshells is considered as a sustainable and environmentally friendly route to produce promising bioceramics such as nano-HAp. Concurrently, decarbonization of eggshells offers the ability to store CO2 as a high value-added Na2CO3 material.

N-acyl hydrazone (NAH) is recognized as a promising framework in drug design due to its versatility, straightforward synthesis, and attractive range of biological activities, including antimicrobial, antitumoral, analgesic, and anti-inflammatory properties. In the global context of increasing resistance of pathogenic bacteria to antibiotics, NAHs represent potential solutions for developing improved treatment alternatives. Therefore, this research introduces six novel derivatives of (EZ)-N\'-benzylidene-2-(6-chloro-9H-carbazol-2-yl)propanehydrazide, synthesized using a microwave-assisted method. In more detail, we joined two pharmacophore fragments in a single molecule, represented by an NSAID-type carprofen structure and a hydrazone-type structure, obtaining a new series of NSAID-N-acyl hydrazone derivatives that were further characterized spectrally using FT-IR, NMR, and HRMS investigations. Additionally, the substances were assessed for their tuberculostatic activity by examining their impact on four strains of M. tuberculosis, including two susceptible to rifampicin (RIF) and isoniazid (INH), one susceptible to RIF and resistant to INH, and one resistant to both RIF and INH. The results of our research highlight the potential of the prepared compounds in fighting against antibiotic-resistant M. tuberculosis strains.

Here, doubly protonated Lindqvist-type niobium oxide cluster [H2(Nb6O19)]6-, fabricated by microwave-assisted hydrothermal synthesis, exhibited superbase catalysis for Knoevenagel and crossed aldol condensation reactions accompanied by activating C-H bond with pKa >26 and proton abstraction from a base indicator with pKa=26.5. Surprisingly, [H2(Nb6O19)]6- exhibited water-tolerant superbase properties for Knoevenagel and crossed aldol condensation reactions in the presence of water, although it is well known that the strong basicity of metal oxides and organic superbase is typically lost by the adsorption of water. Density functional theory calculation revealed that the basic surface oxygens that share the corner of NbO6 units in [H2(Nb6O19)]8- maintained the negative charges even after proton adsorption. This proton capacity and the presence of un-protonated basic sites led to the water tolerance of the superbase catalysis.

Herein, aqueous nitrate (NO3 -) reduction is used to explore composition-selectivity relationships of randomly alloyed ruthenium-palladium nanoparticle catalysts to provide insights into the factors affecting selectivity during this and other industrially relevant catalytic reactions. NO3 - reduction proceeds through nitrite (NO2 -) and then nitric oxide (NO), before diverging to form either dinitrogen (N2) or ammonium (NH4 +) as final products, with N2 preferred in potable water treatment but NH4 + preferred for nitrogen recovery. It is shown that the NO3 - and NO starting feedstocks favor NH4 + formation using Ru-rich catalysts, while Pd-rich catalysts favor N2 formation. Conversely, a NO2 - starting feedstock favors NH4 + at ≈50 atomic-% Ru and selectivity decreases with higher Ru content. Mechanistic differences have been probed using density functional theory (DFT). Results show that, for NO3 - and NO feedstocks, the thermodynamics of the competing pathways for N-H and N-N formation lead to preferential NH4 + or N2 production, respectively, while Ru-rich surfaces are susceptible to poisoning by NO2 - feedstock, which displaces H atoms. This leads to a decrease in overall reduction activity and an increase in selectivity toward N2 production. Together, these results demonstrate the importance of tailoring both the reaction pathway thermodynamics and initial reactant binding energies to control overall reaction selectivity.