Practical Synthesis Research Articles

Practicable Syntheses of Electroluminescent Ionic 2,2′‐Bifluorenes

AbstractThe development of a practicable library synthesis of ionic 2,2′‐bifluorenes is described that improves the safety and reduces waste associated with the ubiquitous method of preparing these and related electroluminescent compounds. Additionally, an X‐ray crystal structure that reveals how triflate counterions can provide a second link between the alkylimidazolium subunits and the photoluminescent core is presented.

Robust Organocatalytic Three-Component Approach to 1,3-Diarylallylidene Pyrazolones via Consecutive Double Condensation Reactions.

A robust pyrrolidine-BzOH salt-catalyzed one-pot three-component reaction involving 4-unsubstituted pyrazolones, aryl/heteroarylaldehydes, and aryl methyl ketones is reported for the first time. This catalytic process fortifies an efficient method, allowing for the practical synthesis of a wide array of synthetically useful 1,3-diarylallylidene pyrazolones in good to high yields exclusively in their single geometrical isomer forms. Furthermore, this catalyst facilitates a sequential double condensation reaction under thermal conditions, thereby enabling two consecutive C═C bonds through displacement of aryl groups. Moreover, this organocatalytic technique achieves a 100% carbon atom economy, marking a significant step forward toward efficient and sustainable synthesis.

The altered landscape as heterotopia

ABSTRACT This paper considers the contemporary photographic practices of the authors, aligning their conceptual ideas and working methodology with notions of heterotopia. It argues for a positioning within contemporary altered landscape photography that considers place as a heterotopia, a networked system or process that modifies and makes an alternative ‘territory’. In dialogue with a range of relevant authors and artists, the paper contextualises heterotopia and altered landscape spaces as layers of both cultural and ecological intervention. It asserts that an artist in a state of mobility, transit and movement, can effectively employ notions of heterotopia to inform a creative photographic practice. We build on existing heterotopologies through the photographic practices of the authors, altered landscape photography by Australian artist Shane Hulbert, and the cultural investigations of expatriation by Greek artist Ioannis Galanopoulos Papavasileiou. The artists, through phenomenology, lens-based practice and noetic synthesis, approach altered landscape photography from two divergent cultural perspectives; one through the lens of postcolonial national imaging, the other through a trans-national experience of expatriation. We propose that both the cultural and geographic counter-site of an altered landscape, and the social and psychological state of expatriation, are informed by notions of heterotopia, and therefore build on existing heterotopologies.

Regioselective Synthesis of Cycloalkane-fused Pyrazolo[4,3-e]pyridines through Tandem Reaction of 5-aminopyrazoles, Cyclic Ketones and Electron-rich Olefins.

Pyrazolopyridines are interesting fused heterocyclic pharmacophores that combine pyrazole and pyridine; two privileged nuclei extensively studied and with a wide range of applications. They can be obtained by a broad variety of synthetic methods among which multicomponent reactions have gained importance, especially from 5-aminopyrazoles and dielectrophilic reagents. However, the search for new approaches more in tune with sustainable chemistry and the use of unconventional heating in three-component synthesis are open and highly relevant study fields. A novel, practical and efficient three-component synthesis of cycloalkane-fused pyrazolo[ 4,3-e]pyridines was developed through a tandem reaction of 5-aminopyrazoles, cyclic ketones and electron-rich olefins, using microwave induction in perfluorinated solvent and iodine as catalyst. The microwave-induced three-component approach applied in this work promoted the construction of 10 new pyrazolopyridines with high speed and excellent control of regioselectivity, favoring the linear product with good yields; where the versatility of electron-rich olefins in iodine-catalyzed cascade heterocyclizations, granted the additional benefit of easy isolation and the possibility to reuse the fluorous phase. Although pyrazolopyridines have been synthetically explored because of their structural and biological properties, most of the reported synthetic methods use common or even toxic organic solvents and conventional heating or multi-step processes. In contrast, this study applied a multicomponent methodology in a single step by microwave induction and with the versatility provided in this case by the use of perfluorinated solvent, which allowed easy isolation of the final product and recovery of the fluorous phase.

ZeoReader: Automated extraction of synthesis steps from zeolite synthesis literature for autonomous experiments

Material synthesis literature documents detailed synthesis procedures, which provide valuable insight and guidance for designing practical synthesis routes. Information extraction (IE) techniques have emerged as powerful tools to obtain structured synthesis-related data. However, current IE methods struggle to differentiate semantically similar experimental records and extract dense experimental properties with abstract expressions, limiting their effectiveness in the zeolite synthesis domain. To this end, we propose ZeoReader, an end-to-end IE framework designed to extract synthesis steps from zeolite synthesis literature. Specifically, to effectively distinguish between semantically similar descriptions of synthesis and characterization experiments, ZeoReader constructs a MatSciBERT-based paragraph classifier that offers rich prior synthesis knowledge. For improving the extraction of complete synthesis steps in complex sentences, ZeoReader develops a two-stage synthesis step extraction model, which introduces customized contrastive learning to model the distributions of dense properties and capture features of abstract expressions. Furthermore, domain-specific parsing strategies are proposed to enable ZeoReader to automatically parse PDF documents, identify synthesis experimental passages, and extract structured zeolite synthesis steps containing actions and corresponding experimental properties. Extensive experiments demonstrate that ZeoReader detects synthesis passages with an accuracy of 94.06% on out-of-sample documents and extracts experimental actions and properties with an F1 score of 93.05% and 74.99%, respectively. Our proposed IE framework can be embedded in autonomous unmanned zeolite synthesis experiments to rapidly understand, reproduce and validate existing experimental routes, thus facilitating new zeolite exploration.

An efficient and practical synthesis of ferroptosis inducer erastin

Erastin, a classic ferroptosis inducer, mediates ferroptosis through various molecular pathways. A highly efficient and convenient synthesis of erastin has been developed, starting from 2-nitrobenzoic acid through 7 steps in an overall yield of 21.6%. This synthesis approach features the efficient construction of the key quinazolinone core and highly selective bromination.

Techniques for using backlighting to enhance the expressiveness of photographs

This article examines the historical and contemporary aspects of backlighting in photography, focusing on its visual and psychological impact and the technical and color features that enhance its effectiveness. Drawing on principles established during the Baroque era by artists like Caravaggio and Rembrandt, the study explores how modern photographers integrate these techniques with advanced lighting technologies and color theories, particularly those of Johannes Itten. Through a comprehensive analysis of backlighting applications in portrait and food photography, the research highlights how this technique enhances depth, texture, and emotional resonance in images. The findings demonstrate that mastery of backlighting, combined with technical proficiency and an understanding of color interactions, allows photographers to create compelling and emotionally impactful works. The novelty of this work lies in its synthesis of historical practices with modern technological advancements, offering new insights into the creative possibilities of backlighting in professional photography.

STRATEGIC PLANNING FOR COMMUNITY ENGAGEMENT IN THE ACTIVITIES OF NON-GOVERNMENTAL ORGANIZATIONS

Strategic planning in the activities of non-governmental organizations is designed to outline guidelines for responding to the needs of the target audience. Organizations of the third sector of Ukraine direct their activities to help the population affected by the war. For example, the Red Cross Society of Ukraine (URCS) seeks to respond to the dynamic humanitarian crisis in Ukraine by adapting its strategic plan to the changing needs of the affected population. The revision of the Strategic Plan for 2026-2030 is aimed at ensuring the relevance, effectiveness and impact of the programs and interventions of the URCS. Therefore, the purpose of this study was to find out the features of strategic planning regarding the involvement of communities in the activities of non-governmental organizations using the example of the Red Cross Society of Ukraine. This goal is achieved through the analysis of domestic and foreign scientific surveys, program documents of the URCS. This study provides a review of the research that provides practical advice for organizations to identify the capacity needed to support community engagement. This article attempts a practical synthesis of how the practice framework defines the needs of an organization's capacity to engage communities, which is necessary to further develop and test these capacities. Among other considerations, such work must take into account the considerable diversity that exists among NGOs. The article also showcases an example of the annual strategic plan of the URCS Community Engagement and Accountability Department for community engagement activities. Nevertheless, it is hoped that these practical observations and ideas will be tested and refined and ultimately lead to a better understanding of how organizations should prepare for optimal community participation.

Transforming Tomorrow: A Practical Synthesis of STEAM and PBL for Empowering Students’ Creative Thinking

Transforming Tomorrow: A Practical Synthesis of STEAM and PBL for Empowering Students’ Creative Thinking

Stable and Recyclable Copper Nanoclusters with Exposed Active Sites for Broad‐Scope Protosilylation in Open Air

Despite recent advances in cluster‐based catalysis for organic synthesis, the substrate scope of reactions catalyzed by metal nanoclusters is typically not superior to previously established catalytic systems. Herein, we develop new atomically precise copper nanoclusters for protosilylation, with scope expanding to alkenes and simple enynes that were not suitable for prior synthetic methodologies with traditional copper complexes. The involvement of a second copper center in the metal kernel during the migratory insertion step is thought to be responsible for the expanded scope. In addition, the reaction is highly compatible with water and can be carried out in open air rather than under inert gas protection. Mechanistic studies suggest that the cluster‐catalyzed protosilylation proceeds in the absence of silyl radicals. The current findings demonstrate the potential of using metal nanoclusters for practical and sustainable chemical synthesis.

Stable and Recyclable Copper Nanoclusters with Exposed Active Sites for Broad-Scope Protosilylation in Open Air.

Despite recent advances in cluster-based catalysis for organic synthesis, the substrate scope of reactions catalyzed by metal nanoclusters is typically not superior to previously established catalytic systems. Herein, we develop new atomically precise copper nanoclusters for protosilylation, with scope expanding to alkenes and simple enynes that were not suitable for prior synthetic methodologies with traditional copper complexes. The involvement of a second copper center in the metal kernel during the migratory insertion step is thought to be responsible for the expanded scope. In addition, the reaction is highly compatible with water and can be carried out in open air rather than under inert gas protection. Mechanistic studies suggest that the cluster-catalyzed protosilylation proceeds in the absence of silyl radicals. The current findings demonstrate the potential of using metal nanoclusters for practical and sustainable chemical synthesis.

Vapor-Solid Interface Synthesis of Highly Crystalline Covalent Triazine Frameworks for Use as Efficient Photocatalysts.

Harsh synthetic conditions for crystalline covalent triazine frameworks (CTFs) and associated limitations on structural diversities impede not only further development of functional CTFs, but also practical large-scale synthesis. Herein, a mild and universal vapor-solid interface synthesis strategy is developed for highly crystalline CTFs employing trifluoromethanesulfonic acid vapor as catalysts. A series of highly ordered simple and functional CTFs (CTF-TJUs) can be facilely produced. In particular, the porphyrin-involved functional CTF (CTF-TJU-Por1) with high crystallinity is synthesized for the first time via this universal approach. The mechanism of vapor-catalyzed trimerization of nitrile monomers is thoroughly investigated through semi in situ characterizations. As a proof of concept, the photocatalytic performance of synthesized CTFs for water splitting is evaluated. CTF-TJU-133 exhibits significantly greater photocatalytic rates for hydrogen (4.35µmolh-1) and oxygen (2.18µmolh-1) evolutions during overall water splitting under visible light irradiations compared to other CTF-TJUs, representing one of the highest values among reported CTF photocatalysts. Further studies reveal that enhanced photocatalytic performance of CTF-TJU-133 results from optimized band structure, extended visible-light absorption, and high carrier separation efficiency. This study provides a promising strategy to synthesize various simple and functional CTFs, which significantly enriched diversities of CTF family for different application purposes.

Efficient Visible‐Light‐Induced π‐Extension of Perylene Tetraesters: An Investigation on Regioselectivity

The present study discloses a highly efficient visible‐light‐induced π‐extension of perylene tetraesters and discussion on the regioselectivity in the photocyclization. We initially found that π‐extension reaction of 3,4‐dimethoxyphenyl perylene tetraester smoothly proceeded by only irradiating blue LED with a complete regioselectivity. Investigations of the photocyclization with various substrates revealed the relationship between the regioselectivity and electron‐donating/withdrawing effects of the substituents on the aromatic groups. Moreover, theoretical investigation suggested the importance of bond alteration in the aromatic groups: cyclization proceeds preferentially at shorter C‐C bonds with higher double bond characters. The findings will open new possibilities for the practical synthesis of custom‐designed π‐extended perylene materials.

Photoinduced Decarboxylative Thioacylation of N-Hydroxyphthalimide Esters with Tetraalkylthiuram Disulfides.

Dithiocarbamate is a key structural sequence in pharmaceuticals and agrochemicals, and its synthesis is crucial in organic chemistry. Although significant progress has been made in related synthesis research, developing a practical and universal synthesis method remains fascinating. Herein, we report a new visible-light-induced decarboxylation coupling reaction between N-hydroxyphthalimide esters and tetraalkylthiuram disulfides, which uses Ir(ppy)3 as a photocatalyst to promote the generation of corresponding decarboxylation thioacylation product-dithiocarbamates in high yields. This redox-neutral protocol uses inexpensive and readily available starting material under mild reaction conditions, exhibiting broad substrate scope and wide functional group compatibility. This method can be further used for post modification of complex natural products and bioactive drugs.

Challenges and perspectives in using unspecific peroxygenases for organic synthesis

In the past 20 years, unspecific peroxygenases (UPOs) have emerged as promising biocatalysts for various organic transformations. Particularly, we have witnessed great attention being paid to the screening of new enzymes and expansion of the substrates/products. However, challenges such as enzyme stability, low turnover numbers, and substrate specificity hinder their widespread utilization in practical organic synthesis. This review article provides a concrete and mini-overview of the challenges associated with using UPOs in organic synthesis and discusses strategies for enzyme engineering to overcome these limitations. The article highlights recent advancements in UPO research and presents potential solutions to enhance their catalytic efficiency, stability, substrate specificity, and regioselectivity. Additionally, the review outlines the current methodologies employed for directed evolution and protein engineering of UPOs, along with computational modeling approaches for rational enzyme design. By addressing the challenges and exploring avenues for enzyme engineering, this review aims to shed light on the prospects of UPOs in organic synthesis.

Practical Synthesis of Macrobicyclic Thiolincosamines.

Scalable syntheses of the northern macrobicyclic thiolincosamine fragments of two structurally complex antibiotic candidates, BT-33 and cresomycin, are presented. A key transformation in each route is the highly diastereoselective addition of a putative allenylzinc nucleophile to a common Ellman sulfinimine intermediate using a zinc-promoted Barbier-type propargylation protocol that is detailed herein. These transformations proceed with dynamic kinetic resolution and use just 1.2 equiv of each respective propargyl bromide precursor.

NaIO4/NH2OH-mediated Efficient Synthesis of Phosphoroamidates from Anilines and Triethyl Phosphite

AbstractA simple, efficient, and metal-free method was developed for the synthesis of phosphoroamidates. In essence, a mixture of sodium periodate (NaIO4) and hydroxylamine (NH2OH⸱HCl) was used in stoichiometric amounts to execute the phosphoramidation reaction of aromatic amines and triethyl phosphites at room temperature, in open air. This method offers a practical synthesis route to afford a diverse range of phosphoroamidates via the construction of P − N bonds, with excellent functional group compatibility and good yields under mild conditions.

Green Approaches to Extractive Metallurgy: A Novel Synthesis of Sustainable Practices

The realm of extractive metallurgy, a cornerstone for diverse industrial applications, has traditionally grappled with environmental challenges stemming from conventional extraction methods. This thorough literature review delves into the realm of innovative green approaches within extractive metallurgy, with the overarching goal of synthesizing sustainable practices. The introduction casts a spotlight on the environmental quandaries associated with traditional metallurgical practices, underscoring the imperative for ecologically friendly alternatives. The research methodology meticulously entails a comprehensive review of peer-reviewed literature, applying stringent criteria to handpick studies that delve into sustainable metallurgical practices. The results and discussion section intricately categorizes and dissects an array of green approaches in metal extraction, including bioleaching, ionic liquids, supercritical fluid extraction, green hydrometallurgy, electrochemical methods, and hybrid processes, providing nuanced insights into their efficacy and sustainability. Through the lens of case studies, the study sheds light on recent strides made by industries that have wholeheartedly embraced these sustainable practices, with a keen focus on unraveling their consequential environmental and economic impacts. Moreover, the study conscientiously addresses the challenges encountered in the adoption of green metallurgy and adeptly identifies latent opportunities for further development in this transformative field. The findings resonate with a resounding call for the widespread adoption of sustainable practices within extractive metallurgy, emphasizing their profound implications for both industrial application and the trajectory of future research endeavors. This expanded exploration underscores the pivotal role of environmentally conscious approaches in reshaping the landscape of extractive metallurgy, paving the way for a more sustainable and responsible future.

Scalable ammonia synthesis on the modified crystal structure of Cu3PS4 electrocatalyst

Ammonia production, which is vital for agricultural and industrial applications, typically relies on energy-intensive processes that contribute to global CO2 emissions. Electrochemical nitrogen reduction is a promising alternative, although it faces challenges such as low yield and selectivity. Transition-metal-based catalysts, particularly Cu, are promising for overcoming these limitations. Cu3PS4 catalysts were synthesized and evaluated using a 9 cm2-scale electrode, revealing enhanced performance attributed to change in the crystal and electronic structure of Cu, facilitating N2 adsorption and improving the reaction activity. Notably, the ammonia synthesis rate reached 128 μg h-1 mgcat-1 at −1.0 V vs. RHE and faradaic efficiency was 34 % at −0.8 V vs. RHE. These findings provide potential insights into the improvement of practical electrochemical synthesis of ammonia.

Biomedical applications of terbium oxide nanoparticles by Couroupita guianensis aubl leaves extract: A greener approach

Couroupita guianensis aubl (CGA) is a plant known for its therapeutic characteristics and extensively used in biomedicine. This paper presents a method for synthesizing terbium oxide (Tb2O3) nanoparticles (NPs) utilizing the leaves extract of CGA which is sustainable and environmentally friendly. The practical synthesis of Tb2O3 NPs was validated using UV–vis analysis, revealing a prominent peak at 246 nm and the calculated band gap value of 3.02 eV. The existence of numerous functional groups and molecular bonding interactions in the Tb2O3 NPs was confirmed using FTIR spectrum analysis. In addition, the XRD examination confirmed that the nanoparticles had a crystalline structure with dimensions of 27.3 nm. The TEM imaging revealed the particle size of around 5.63 nm. The manufactured Tb2O3 NPs were analysed for anticancer capabilities against human MCF-7 cancer cell lines. Overall, our study emphasizes the ability of green-produced Tb2O3 NPs to be versatile agents with antidiabetic, antioxidant, and anticancer effects. These nanoparticles are potentially used in biomedical applications, providing long-lasting solutions to various health-related problems.