Search Results (1,955)

Di(hetero) aryl and alicyclic amine derivatives of thieno[2,3-b]pyridine were synthesized in good to high yields (45–76%) via palladium-catalyzed Buchwald–Hartwig amination. The reactions were performed using methyl 5-bromothieno[2,3-b]pyridine-2-carboxylate, prepared in this work, and a variety of substituted anilines bearing either electron-donating groups (EDGs) or electron-withdrawing groups (EWGs), as well as pyridinyl amines, and saturated heterocyclic amines such as morpholine and piperidine. For most substrates, the optimal conditions involved Pd(OAc)₂, rac-BINAP, and Cs₂CO₃ in toluene at 100 °C under argon. Substrate bearing EWGs and electron-deficient pyridinyl amines required Xantphos as the ligand, while reactions with piperidine were only successful using Pd₂(dba)₃ as a palladium (0) source. The antiparasitic activity of the synthesized compounds was evaluated against Trypanosoma brucei (T. brucei) and Leishmania infantum (L. infantum) in both promastigote and amastigote forms. Most compounds exhibited no significant cytotoxicity (CC₅₀ > 100 μM) in PMA-differentiated THP-1 derived macrophage cells. Analysis of substituent effects focusing on the nature of amino substitution at position C(5) revealed distinct trends in antiparasitic activity. Notably, one compound exhibited activity against Leishmania infantum promastigotes that was nearly four times higher than that of the reference drug miltefosine, and its selectivity index was also approximately fourfold higher. Full article

Squalene and squalane are widely used cosmetic ingredients valued for their emollient properties and excellent skin compatibility, yet sustainable sourcing remains a challenge. This study presents an integrated and eco-friendly strategy for valorizing wine lees as a renewable source of squalene and converting it into stable, high-performance squalane. Squalene was efficiently recovered from yeast-rich winery waste through optimized ultrasound-assisted extraction, followed by chromatographic purification. Green catalytic hydrogenation using palladium supported on natural clay minerals enabled the selective conversion of squalene into squalane under mild conditions. The functional evaluation via in vitro transport studies across an artificial membrane, using quercetin as a poorly permeable model antioxidant, demonstrated enhanced permeation compared with conventional vehicles, while accelerated aging experiments further confirmed the superior oxidative stability of squalane relative to native squalene. Overall, this work provides a proof of concept for upcycling winery by-products into multifunctional cosmetic ingredients that combine sustainability, stability, and functional performance, supporting circular economy principles and the growing demand for ethically sourced raw materials in the cosmetic industry. Full article

The creation of new potential metal-based therapeutics largely relies on the development of useful ligand scaffolds. In recent years, our research group has introduced thiophosphoryl-functionalized carboxamides as a convenient framework for obtaining biologically active cyclopalladated derivatives. In continuation of these studies, β-(aminoalkyl)phosphine sulfides bearing additional substituents in the ethylene backbone were synthesized for the first time and reacted with picolinic acid to afford a series of new functionalized amide ligands. The latter readily underwent direct cyclopalladation under the action of PdCl₂(NCPh)₂ under mild reaction conditions. The resulting S,N,N-complexes were studied for in vitro cytotoxicity against several solid and hematopoietic cancer cell lines, as well apoptosis induction and DNA damage ability, which showed their promising anticancer properties. In addition, moderate antibacterial activity was observed for a representative palladocycle of the β-thiophosphorylated derivatives. Full article

Chromite beneficiation tailings (CBTs) represent a significant environmental challenge, while simultaneously containing valuable metals that remain largely unrecovered. In this study, a sequential thermochemical–hydrometallurgical route was investigated for selective chromium extraction and the enrichment of platinum group metals (PGMs) from CBTs generated at the Donskoy Mining and Processing Plant. Alkaline sintering with Na₂CO₃ at 1000 °C followed by aqueous leaching enabled the transfer of up to 98%–99% of chromium into solution. The resulting residue was enriched in non-ferrous metals, rare earth elements, and PGMs. Subsequent sulfation roasting and water leaching promoted the dissolution of magnesium, nickel, and rare earth elements, while platinum and palladium remained predominantly in the solid phase, due to their low solubility under the applied conditions. Microstructural analysis using SEM–EPMA revealed that PGMs are selectively concentrated in Ni-bearing micro-inclusions, with local platinum content reaching up to 3.8 wt.% in Ni-rich regions. The proposed sequential processing strategy enables efficient chromium recovery and significant PGM enrichment in the residual phase, demonstrating the potential of CBTs as a secondary resource for integrated metal recovery. Full article

Environmental contamination by persistent industrial dyes such as Amido Black demands highly efficient photocatalysts for advanced water treatment. Structural, chemical, and optical strategies based on TiO₂ nanotube engineering are widely explored for this purpose. In this work, highly ordered TiO₂ nanotube arrays were fabricated by electrochemical anodization and subsequently decorated with Pd nanoparticles via potentiostatic electrodeposition (10–300 s), enabling precise control of Pd nanoparticle size and loading. The resulting materials were systematically characterized by SEM, TEM, XRD, XPS, UV–vis DRS, and PL spectroscopy, and their properties were correlated with the photocatalytic degradation of Amido Black under both UV and visible light irradiation. The study reveals a clear size-dependent duality in the role of Pd. For intermediate Pd nanoparticles (≈9 nm, 20 s), Pd behaves predominantly as an electron sink, forming an efficient Schottky junction with anatase TiO₂ that markedly suppresses charge carrier recombination. This configuration yields ≈ 97% Amido Black removal after 120 min of UV irradiation, with an apparent rate constant about three times higher than that of bare TiO₂ nanotubes. In contrast, for ultra-small Pd nanoparticles (≈6 nm, 10 s), interfacial defect states sensitize TiO₂ to visible light, enabling ≈ 65% degradation after 270 min and a rate constant roughly four times higher than that of undecorated nanotubes under visible illumination. At long deposition times (≥150 s), Pd agglomeration leads to enhanced photoluminescence and markedly reduced photocatalytic activity, indicating increased recombination and less effective utilization of photogenerated charges. This provides a practical design rule to rationally tailor Pd–TiO₂ nanotube photocatalysts for targeted UV or visible light applications in dye removal and broader environmental remediation scenarios Full article

Platinum group metals (PGMs), platinum (Pt), palladium (Pd) and rhodium (Rh), are critical for automotive emission control, chemical manufacturing and emerging energy technologies, yet their supply is limited and geographically concentrated. Their designation as critical raw materials (CRMs) in the EU has intensified recycling efforts, especially from spent automotive catalysts. Conventional pyrometallurgical and acid-based hydrometallurgical routes achieve high recovery efficiencies but rely on aggressive reagents and energy-intensive processing. Deep eutectic solvents (DESs) have emerged as greener leaching media capable of dissolving PGMs under milder and tunable conditions. This review outlines the conventional hydrometallurgical framework, summarizes DES fundamentals relevant to metals dissolution, and critically assesses recent advances in DES-based leaching of PGMs from spent catalysts. The influence of solvent composition, oxidants and complexing ligands on PGMs speciation and recovery is discussed, together with emerging reporting guidelines and research priorities. Overall, DES-based leaching offers a promising and potentially safer route for autocatalyst recycling but the technology remains at an early stage of development, requiring further mechanistic insight and sustainability evaluation. Full article

Pyrrolo[2,3-d]pyrimidine is a privileged fused heterocyclic scaffold that has attracted considerable attention in medicinal chemistry due to its diverse biological activities. Herein, we report an efficient synthesis strategy for the preparation of the pyrrolo[2,3-d]pyrimidine-based natural toyocamycin aglycone and pyrrolo[2,3-d]pyrimidine derivatives. The synthesis of toyocamycin aglycone features a key benzylamine nucleophilic substitution followed by a palladium-catalyzed cyanation reaction. From a key intermediate derived from this route, nineteen new pyrrolo[2,3-d]pyrimidine derivatives were rapidly synthesized via key Suzuki–Miyaura coupling and amine nucleophilic substitution reactions. Their cytotoxic activities were evaluated against Huh-7 and HepG liver cancer cell lines. Most derivatives were inactive after 24 h. However, 28a–28c, 28e and 28f exhibited moderate cytotoxicity with IC₅₀ values ranging from 5.7 to 62.6 μM. Among them, compound 28e displayed the highest potency against HepG cells, with IC₅₀ values of 5.7 μM. Compared with normal HEK293 cells, it showed a selectivity index (SI) of 3.60 against HepG cells. Preliminary structure-activity relationship analysis suggested that incorporation of a cyclopropyl group further improves antitumor activity. Full article

Plating on Plastics (PoP) requires specific surface pre-treatment steps to enable metallization. The conventional PoP industry utilizes hexavalent chromium (toxic, carcinogenic) and palladium (critical raw material) for surface etching and activation, respectively, raising significant health, environmental, and economic concerns. This work is based on a new Cr⁶⁺-free and Pd-free PoP technology that uses piranha (H₂O₂-H₂SO₄) solutions for surface etching, nickel salts for activation, and NaBH₄ for reduction, ultimately forming metallic nucleation sites for downstream electroless plating and electroplating. A comprehensive modeling approach was developed to simulate and predict unit operation performance (reaction kinetics and yields) and material properties (contact angle and adhesion) across processing stages of the new technology. State-of-the-art and data-driven modeling revealed the combinatorial relationships among process performance, the achieved properties and the different settings of process operating conditions. The results also highlighted capabilities for tuning all processes over a range of conditions, reaching desired product specifications (adhesion and thickness). The models were constructed as a Decision Support Tool (DST) serving economic, environmental, safety and Safe and Sustainable by Design (SSbD) objectives. The DST can be used through a user-friendly interface that enables the insertion of user-defined inputs and monitoring of optimization results. Full article

We engineered a compact methanol steam reforming (MSR) system tailored to power a 1 kW High-Temperature Proton Exchange Membrane (HT-PEM) fuel cell. The unit integrates an evaporator, reformer, and burner within a cylindrical titanium-alloy vacuum flask to minimize parasitic heat loss. Guided by an Artificial Intelligence Complex System Response (AICSR) framework, we developed a segmented catalyst architecture that positions an optimized Pd/ZnO/Al₂O₃ catalyst downstream of a commercial Cu–Zn catalyst bed. This spatial configuration reduces palladium consumption by >50% while maintaining a hydrogen generation rate of 8000 sccm at 250 °C. During a 40 h stability test, the system exhibited a low deactivation rate of 0.235% h⁻¹, with methanol conversion decaying gradually from 98.1% to 88.7%. The downstream PdZn intermetallic phase actively promoted the water–gas shift (WGS) reaction, restricting CO concentration to an average of 3.9% (minimum 2.5%). Achieving a system thermal efficiency of 88.589% and a 20 min startup time, this design validates AI-assisted spatial catalyst distribution as a highly viable strategy for compact hydrogen generation. Full article

Treatment of palladium precursor Pd(PPh₃)Cl₂ with equivalent arylfluorodithiophosphato ligand [PPh₄][(4-EtO-C₆H₄)FPS₂] in chloroform at reflux resulted in a mononuclear palladium(I)–sulfur complex cis-[Pd(PPh₃)₂{κ²-S,S′-(4-EtO-C₆H₄)FPS₂}]. This complex was characterized by UV-Vis and IR spectroscopic analysis, thermogravimetric analysis, and XPS analysis, and its molecular structure has been established by single-crystal X-ray diffraction. SBA-15, as a mesoporous material, was selected as a mesoporous silica substrate to further form a homogeneous catalyst, Pd@SBA-15, which has been characterized by IR spectroscopy, electron microscope and N₂ adsorption–desorption test. In addition, the catalytic activity of Pd@SBA-15 for the Suzuki–Miyaura cross-coupling reaction was also investigated. Full article

A novel multidentate ligand with an O,N,O-tridentate ligand moiety and an N-heterocyclic carbene (NHC) was synthesized. Its palladium complex, in which the NHC part coordinates to the palladium atom, was synthesized and structurally characterized. The O,N,O-part coordinated to an early transition metal such as titanium. The Ti-Pd heterobimetallic complex was observed in solution. Full article

Green synthesis of nanoparticles has become one of the most popular research areas in recent decades due to its environmentally friendly nature and the minimization of harmful chemical by-products. This review focuses on the mechanism of palladium nanoparticle (PdNP) biosynthesis using bacteria, fungi, algae, and plants, and their potential biological activities, such as antibacterial, anticancer, antioxidant, and other properties, with the aim of their further biomedical applications. The role of various biomolecules in these processes is also discussed. Full article

Platinum group elements (PGE) are six rare highly siderophile metals which have similar chemical characteristics and occur together in mineral deposits: platinum (Pt), palladium (Pd), rhodium (Rh), ruthenium (Ru), iridium (Ir) and osmium (Os). In nature, they tend to exist in a metallic state or bond with sulfur and arsenic and occur as trace accessory minerals predominantly in mafic and ultramafic rocks. High industrial demand together with their scarcity in crustal rocks has been reflected in their inclusion in 2025 US Government’s List of Critical Minerals, European Union’s List of Critical Raw Materials and Mongolian List of 11 Critical Minerals. Although Mongolia is not currently a producer, it hosts four types of potentially economic PGE deposits: (1) Podiform chromitites associated with ophiolites; (2) Ni-Cu-PGE sulfide mineralization of rift-related mafic–ultramafic intrusions; (3) Alaskan–Uralian type arc related zoned mafic–ultramafic intrusions; and (4) Placers. Particularly promising are Permian Ni-Cu-PGE sulfide bearing mafic–ultramafic intrusions of the Khangai large igneous province which bear resemblance to mineralized Permian intrusions in Russia (e.g., Norilsk-Talnakh) and N.W. China (e.g., Kalatongke; Tarim basin). In addition, sub-economic ophiolite-hosted PGE mineralization can be extracted as a by-product during chromite mining. There is also the potential for PGE recovery as a by-product in existing gold placer operations in areas hosting ophiolitic massifs and Alaskan–Uralian type intrusions. Mongolia is a promising frontier for PGE exploration and mining. Full article

Pyrrole derivatives are natural organic molecules that are important to the pharmaceutical industry due to their occurrence in nature and their use in a wide range of medical applications. In general, non-symmetric, 1,2,5-triaryl-substituted pyrroles are prepared either by Paal–Knorr condensation or cycloaddition that present synthetic challenges particularly if late-stage functionalization is required. The present study describes a modular approach to synthesizing 1,2,5-triarylpyrroles containing three different arene substituents. Using pyrrole ester building blocks, a sequence of decarboxylative cross-coupling and C–H arylation provides unsymmetrical 1,2,5-triarylpyrroles in a regioselective, stepwise manner; the scope and limitations of the sequence are disclosed. Full article