Article
Green & Sustainable Science & Technology
David Carvajal, Ramon Arcas, Camilo A. Mesa, Sixto Gimenez, Francisco Fabregat-Santiago, Elena Mas-Marza
Summary: This article focuses on the electrochemical reduction and hydrogenation of nitrobenzene to aniline using Cu/Pd electrodes. The study found that the deposition of Pd on the surface of the Cu electrode can decrease the overpotential for nitrobenzene reduction and improve the rate and selectivity of aniline production. Impedance spectroscopy analysis indicates that Pd enhances the production of H* radicals, which are necessary for the nitrobenzene reduction process.
ADVANCED SUSTAINABLE SYSTEMS
(2022)
Review
Chemistry, Physical
Claudia Carlucci
Summary: This article discusses the production of biodiesel using different catalytic methods, such as acids, bases, enzymes or supercritical fluids. Continuous flow processes and microreactors provide better control over experimental variables, increasing efficiency and safety. Additionally, combining other technologies such as microwave irradiation or ultrasounds allows for automation of the production process.
Article
Chemistry, Physical
Jordi Ballesteros-Soberanas, Antonio Leyva-Perez
Summary: We demonstrate that palladium on carbon (Pd/C), a widely available supported Pd catalyst, becomes a selective catalyst after the addition of catalytic amounts of commercially available electron-poor phosphines in the semihydrogenation reaction of alkynes. The catalytic activity is <= 7 times greater, and the selectivity is comparable to that of the industrial benchmark Lindlar catalyst.
JOURNAL OF PHYSICAL CHEMISTRY LETTERS
(2023)
Article
Chemistry, Applied
Filiz Yilmaz, Deniz Hur
Summary: The study successfully synthesized and characterized new palladium complexes, investigating their catalytic activity in the hydrogenation of alkenes under continuous flow conditions. These complexes exhibit high activity and can be reused for multiple cycles.
APPLIED ORGANOMETALLIC CHEMISTRY
(2021)
Article
Chemistry, Physical
Wiyanti F. Simanullang, Jiamin Ma, Ken-ichi Shimizu, Shinya Furukawa
Summary: A silica-decoration methodology was used to enhance the catalytic performance of a Ni-Zn alloy, resulting in high acetylene conversion and ethylene selectivity at 200 degrees Celsius.
CATALYSIS SCIENCE & TECHNOLOGY
(2021)
Article
Chemistry, Physical
Jingpeng Li, Rumin Ma, Sisi Yao, Daochun Qin, Yun Lu, Yuhe Chen, Zehui Jiang, Dongjiang Yang
Summary: Plant-based flow microreactors with bamboo microchannels containing mesoporous TiO2-encapsulating ultrafine Pd nanoparticles were synthesized for continuous-flow hydrogenation. The design of the reactor enables high efficiency (>97%) and excellent stability (1,000 h) due to the abundant oxygen vacancies and open cavities provided by the TiO2 films, which facilitate the growth of Pd nanoparticles and improve their dispersion and catalytic activity. The optimized reactor shows promising potential for Pd-catalyzed hydrogenation in various conditions.
Article
Materials Science, Multidisciplinary
Peng Yin, Ming-Xi Chen, Ming Zuo, Le-Le Zhang, Hai-Wei Liang
Summary: Atomically ordered intermetallic compounds (IMCs) have been synthesized with average particle sizes of < 4 nm by a general synthesis strategy based on the strong chemical interaction between metal and sulfur. These Rh-based IMC catalysts showed enhanced catalytic performance for nitroarene hydrogenation, highlighting the advantages of atomically order structure of IMCs for the chemoselective molecular recognition of nitro groups through geometric and electronic effects.
ACS MATERIALS LETTERS
(2022)
Article
Materials Science, Multidisciplinary
Peng Yin, Ming-Xi Chen, Ming Zuo, Le-Le Zhang, Hai-Wei Liang
Summary: Atomically ordered intermetallic compounds (IMCs) have unique electronic and geometric features that have sparked continuous research interest in catalysis. A general synthesis strategy has been developed to prepare a family of 10 different Rh-based IMCs with average particle sizes of <4 nm, which show enhanced catalytic performance for nitroarene hydrogenation. The atomically ordered structure of IMCs demonstrates advantages in chemoselective molecular recognition of nitro groups through geometric and electronic effects.
ACS MATERIALS LETTERS
(2022)
Article
Chemistry, Multidisciplinary
Guoqiang Zhao, Tian Liu, Binbin Wu, Baoliang Chen, Chiheng Chu
Summary: This study introduces a hierarchically ordered porous poly(2,6-diaminopyridine) (PDAP) as a Pd nanoparticle support for hydrogenation removal of recalcitrant pollutants in water purification. The PDAP support acts as a sorbent and microreactor to enhance the proximity of targeted water pollutants and reactive hydrogen atom species, achieving unprecedently high water purification efficiency. The high activity and in situ regenerativity achieved by rational construction of the support structure sheds light on a new approach for designing efficient and robust heterogeneous hydrogenation catalysts.
ADVANCED FUNCTIONAL MATERIALS
(2021)
Review
Biochemistry & Molecular Biology
Shruti Goel, Mihir Khulbe, Anshul Aggarwal, Abha Kathuria
Summary: Flow chemistry is emerging as a significant technology in organic synthesis, with its miniaturized protocol and advantages of combined techniques leading to improved synthesis and preparation of heterocyclic compounds.
MOLECULAR DIVERSITY
(2022)
Article
Chemistry, Multidisciplinary
Suyong Han, Mahdi Ramezani, Patrick TomHon, Kameel Abdel-Latif, Robert W. Epps, Thomas Theis, Milad Abolhasani
Summary: This study explores the feasibility of utilizing and recovering green solvents with switchable hydrophilicity solvents, presenting an intensified continuous flow strategy and providing accurate in situ reaction monitoring and a scalable green solvent extraction route.
Article
Chemistry, Applied
A. Pla-Hernandez, J. L. Cerrillo, F. Rey, A. E. Palomares
Summary: Pt and Pd catalysts supported on alumina were tested and characterized for the hydrogenation of chlorates. Pt catalysts showed better results and their activity depended on the metal precursor used and calcination temperature, affecting the dispersion of platinum on the alumina surface. The optimized catalyst exhibited stability and simultaneous reduction activity towards chlorate, chlorite, and bromate in water.
Article
Engineering, Environmental
Yingxin He, Naeema Cheshomi, Shane M. Lawson, Arun K. Itta, Fateme Rezaei, Shubhender Kapila, Ali A. Rownaghi
Summary: Catalytically active asymmetric membranes were developed by fixing palladium nanoparticles onto the surface through a specific method, achieving successful hydrogenation of 4-nitrophenol. The newly developed continuous flow hydrogenation module demonstrated good operational stability and high efficiency.
CHEMICAL ENGINEERING JOURNAL
(2021)
Article
Chemistry, Multidisciplinary
Marc Escriba-Gelonch, Jodie Bricout, Volker Hessel
Summary: The research applies circular economy principles to a flow chemistry process for synthesizing vitamin D-3, achieving efficient recycling of starting materials through a novel separation technique using acetonitrile. The study enhances material circularity metrics and demonstrates the potential for sustainable pharmaceutical production processes.
ACS SUSTAINABLE CHEMISTRY & ENGINEERING
(2021)
Article
Engineering, Environmental
Ziqiang Wang, Zechuan Dai, Shengqi Wang, Hugang Zhang, Wenjing Tian, You Xu, Xiaonian Li, Liang Wang, Hongjing Wang
Summary: PdH0.43 NRs prepared by hydrogenating Pd NRs show excellent performance in electrochemical ammonia synthesis, exhibiting high NH3 yield, Faradaic efficiency, and long-term electrochemical stability. This hydrogenation strategy provides a new approach for designing efficient and stable metal hydrides for active NRR.
CHEMICAL ENGINEERING JOURNAL
(2021)
Article
Chemistry, Applied
Steven Ley, Yiding Chen, Alan Robinson, Benjamin Otter, Edouard Godineau, Claudio Battilocchio
Summary: The agrochemical sector faces massive constraints in cost-effective and sustainable production at an increasing scale within a highly complex environment. The application of flow chemistry technology can offer clear advantages in chemical processes, especially in the early stages of R&D for agrochemicals. The value of flow chemistry for businesses is evident, and the number of reported examples in the literature is expected to continue increasing in the agrochemical industry.
ORGANIC PROCESS RESEARCH & DEVELOPMENT
(2021)
Article
Multidisciplinary Sciences
Sougata Roy, James Sipthorp, Bidesh Mahata, Jhuma Pramanik, Marco L. Hennrich, Anne-Claude Gavin, Steven Ley, Sarah A. Teichmann
Summary: This study investigates the role of pregnenolone in prostate cancer and immune cells, suggesting that pregnenolone may promote the development of castration-resistant prostate cancer while also regulating CD8(+) T cell function.
Article
Chemistry, Organic
Oliver M. Griffiths, Henrique A. Esteves, Yiding Chen, Karin Sowa, Oliver S. May, Peter Morse, David C. Blakemore, Steven Ley
Summary: Executing photoredox reactions in flow can improve reaction concentration, reduce reaction time, achieve better yields, facilitate catalyst preparation, and expand substrate scope, demonstrating broad applicability.
JOURNAL OF ORGANIC CHEMISTRY
(2021)
Article
Chemistry, Applied
Guido Gambacorta, Ian R. Baxendale
Summary: In this study, a continuous-flow preparation of 2-benzoxazolinone via the Hofmann rearrangement of salicylamide using trichloroisocyanuric acid as the chlorinating agent was implemented. The system was optimized to avoid solid accumulation and enable the production of large quantities of pure desired material. Additionally, a TCCA-based chlorination of 2-benzoxazolone to the corresponding 5-chloro derivative was carried out under batch conditions.
ORGANIC PROCESS RESEARCH & DEVELOPMENT
(2022)
Article
Chemistry, Multidisciplinary
Pia Mueller, Adam D. Clayton, Jamie Manson, Samuel Riley, Oliver S. May, Norman Govan, Stuart Notman, Steven Ley, Thomas W. Chamberlain, Richard A. Bourne
Summary: The study compared the performance of four different multi-objective optimisation algorithms in chemical reaction optimisation, finding that EIMEGO achieved the highest hypervolume with the lowest number of experiments, while TSEMO performed better in cases with three objectives.
REACTION CHEMISTRY & ENGINEERING
(2022)
Article
Chemistry, Organic
Ben M. J. Lancaster, Alexander J. Nicholls, Ian R. Baxendale
Summary: This communication describes an unprecedented substitution cascade, in which 4-methylpyridine acts as a carbon nucleophile in an unusual SNAr process to form a novel triarylmethane structure. The proposed mechanism is supported by single crystal X-ray analysis, highlighting the efficient synthesis of complex triarylmethane architectures with both substituted phenyl and pyridyl aromatics in a single step.
Article
Chemistry, Organic
Alexander J. Nicholls, Ian R. Baxendale
Summary: This short note describes the synthesis of an amorphous benzo[1,2,3]dithiazole chloride salt, commonly known as Herz salt, using the Herz reaction. The conversions of this species to various useful adducts in medicinal and materials chemistry have been well established, but isolation examples in the literature and characterization data are limited. For the first time, this study provides mass spectrometry data for this compound and proposes a new mechanism of its formation based on new experimental observations and data.
Article
Materials Science, Multidisciplinary
Te Hu, Ian R. Baxendale, Yuchang Su, Fangjiang Li, Shaomi Duan, Yaping Zhang, Honxin Fan
Summary: Combining XRD pattern analysis with DSC curves and thermodynamic equations can optimize the preparation conditions of nanomaterials and improve the speed of the preparation scheme.
APPLIED PHYSICS A-MATERIALS SCIENCE & PROCESSING
(2022)
Article
Chemistry, Organic
Oliver M. Griffiths, Steven V. Ley
Summary: The photocatalytic generation of N-centered radicals has been employed for the synthesis of N-heterospirocycles, offering a reliable method for the construction of beta-spirocydic pyrrolidines from N-allylsulfonamides and alkenes. This study demonstrates the successful construction of various beta-spirocyclic pyrrolidines, including drug derivatives, with moderate to very good yields. Derivatization of the products and a viable scale-up procedure using flow chemistry techniques have also been achieved.
JOURNAL OF ORGANIC CHEMISTRY
(2022)
Article
Chemistry, Organic
James S. Sharley, Guido Gambacorta, Ana Maria Collado Perez, Estela Espinos Ferri, Amadeo Fernandez Miranda, Jorge Sanchez Quesada, Ian R. Baxendale
Summary: In this study, a process for the synthesis of cyclic allylic nitro compounds using greener solvent and lower cost, more robust catalyst was developed. The optimized conditions were able to selectively synthesize important fragrance intermediates such as alpha-dehydroherbac, demonstrating their scope and utility.
Article
Chemistry, Organic
James S. Sharley, Guido Gambacorta, Ana Maria Collado Perez, Estela Espinos Ferri, Amadeo Fernandez Miranda, Isabelle Fernandez Fernandez, Jorge Sanchez Quesada, Ian R. Baxendale
Summary: A new method for the oxidation of Hedione 1 to dehydrohedione 2 has been developed based on a one-pot alpha-chlorination-elimination sequence, which allows for easy scalability. The unprecedented spontaneous elimination of alpha-chloro in methanol enables the oxidation to be carried out as a one-pot protocol, eliminating the need for multiple steps/reactions. A continuous flow process utilizing sulfuryl chloride has also been demonstrated, providing a steady and safe evolution of SO2 gas during the reaction.
Article
Chemistry, Multidisciplinary
Pia Mueller, Aikaterini Vriza, Adam D. Clayton, Oliver S. May, Norman Govan, Stuart Notman, Steven V. Ley, Thomas W. Chamberlain, Richard A. Bourne
Summary: Automated platforms enable fast and efficient optimization of chemical systems with single and multiple objectives. In this study, we demonstrate the application of automated optimization platforms for chemical screening of sulfide oxidations in flow. The identification of unique optima for each substrate emphasizes the importance of rapid and individual experimental optimization for successful compound screening.
REACTION CHEMISTRY & ENGINEERING
(2023)
Article
Multidisciplinary Sciences
James S. Sharley, Guido Gambacorta, Ana Maria Collado Perez, Estela Espinos Ferri, Amadeo Fernandez Miranda, Jorge Sanchez Quesada, Ian R. Baxendale
Summary: This article presents a dataset of spectroscopic analysis performed on starting materials, intermediates, and products related to the synthesis of Hedione. The data was collected at Durham university between October 2020 and September 2021 for the development of a preparative method to Dehydrohedione. The proton, Carbon-13, and Fluorine-19 Nuclear magnetic resonance spectra of the compounds were recorded using Varian 600 MHz and Bruker Avance-40 0 instruments. The IR spectra were recorded using a Perkin Elmer Spectrum Two UATR Two FT-IR instrument, and accurate mass measurement was performed using a Waters QtoF premier mass spectrometer.
Article
Chemistry, Multidisciplinary
Samuel L. Bourne, Franz Amann, Steven V. Ley
Summary: This article provides an overview of the factors contributing to the rise of flow chemistry in the pharmaceutical industry over the past two decades. It highlights the challenges faced by the industry and how scientific progress has helped to overcome them. Current trends and examples of progress at CARBOGEN AMCIS are discussed, giving a speculative glimpse into the future of drug development and manufacturing.
Article
Chemistry, Multidisciplinary
Ricardo Labes, Julio C. Pastre, Richard J. Ingham, Claudio Battilocchio, Henrique M. Marcon, Mariana C. F. C. B. Damiao, Duc N. Tran, Steven V. Ley
Summary: This study reports the rapid synthesis of 2-pyrazolines from aldehydes via [3 + 2] cycloaddition of unstabilised diazo species and mono and di-substituted alkenes. The development includes semi-continuous and fully continuous methods, with a fully automated compound library generation and a graphical interface for automation control.
REACTION CHEMISTRY & ENGINEERING
(2023)
