Organic Process Research & Development最新文献_第8页

Study on Continuous-Flow Process for Direct Synthesis of p-Aminophenol from Nitrobenzene 从硝基苯直接合成对氨基苯酚的连续流工艺研究

IF 3.1 3区化学

Organic Process Research & Development Pub Date : 2024-09-11 DOI: 10.1021/acs.oprd.4c0027510.1021/acs.oprd.4c00275

Jinpeng Huang, Changlu Zhou, Chunping Li and Zhong Xin*,

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引用次数: 0

PAT Aided Feasibility Study on Continuous Crystallization of Benzotriazole 苯并三唑连续结晶的 PAT 辅助可行性研究

IF 3.4 3区化学

Organic Process Research & Development Pub Date : 2024-09-11 DOI: 10.1021/acs.oprd.4c00201

Yang Zhang, Lu Zhang, Guangzheng Zhou, Jian Heng, Xue Zhong Wang

{"title":"PAT Aided Feasibility Study on Continuous Crystallization of Benzotriazole","authors":"Yang Zhang, Lu Zhang, Guangzheng Zhou, Jian Heng, Xue Zhong Wang","doi":"10.1021/acs.oprd.4c00201","DOIUrl":"https://doi.org/10.1021/acs.oprd.4c00201","url":null,"abstract":"As an important fine chemical with a wide range of applications, benzotriazole has traditionally been purified by batch crystallization. Batch operation has some potential known disadvantages compared with continuous mode operation, including batch-to-batch variations, the need for large inventories, and being more challenging to process control. In this feasibility study, continuous mixed-suspension-mixed-product removal (MSMPR) crystallization is investigated for benzotriazole purification with the support of online microscopic imaging and attenuated total reflectance ultraviolet (ATR-UV) spectroscopy. The metastable zone width is determined by the in situ imaging method, and the growth rate of needle-shaped crystals is found to be independent of their dimensions. The ATR-UV spectroscopy is utilized to provide real-time concentration measurements with a calibration model established by a chemometric method. The steady state of the crystallization process is online-identified by spectrum analysis, which always becomes stable around 7–8 residence times, regardless of initial solution concentration and residence time. The optimum process parameters of continuous crystallization are determined according to the product yield and particle size distribution.","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2024-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142166488","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Study on Continuous-Flow Process for Direct Synthesis of p-Aminophenol from Nitrobenzene 从硝基苯直接合成对氨基苯酚的连续流工艺研究

IF 3.4 3区化学

Organic Process Research & Development Pub Date : 2024-09-11 DOI: 10.1021/acs.oprd.4c00275

Jinpeng Huang, Changlu Zhou, Chunping Li, Zhong Xin

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引用次数: 0

PAT Aided Feasibility Study on Continuous Crystallization of Benzotriazole 苯并三唑连续结晶的 PAT 辅助可行性研究

IF 3.1 3区化学

Organic Process Research & Development Pub Date : 2024-09-11 DOI: 10.1021/acs.oprd.4c0020110.1021/acs.oprd.4c00201

Yang Zhang, Lu Zhang, Guangzheng Zhou*, Jian Heng and Xue Zhong Wang*,

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引用次数: 0

Green Chemistry Articles of Interest to the Pharmaceutical Industry 制药业感兴趣的绿色化学文章

IF 3.4 3区化学

Organic Process Research & Development Pub Date : 2024-09-10 DOI: 10.1021/acs.oprd.4c00300

Melissa A. Ashley, Miles H. Aukland, Marian C. Bryan, Megan A. Cismesia, Theresa Dutschei, Oliver D. Engl, Pascal S. Engl, Álvaro Enriquez Garcia, Vanessa Harawa, George Karageorgis, Christopher B. Kelly, Alexandre Leclair, Johnny W. Lee, Zhen Lei, Wei Li, Jan Pawlas, Paul F. Richardson, Samuel C. Scott, Alan Steven, Balaram S. Takale, Dauzhan Yerkozhanov, Mingshuo Zeng

引用次数: 0

Green Chemistry Articles of Interest to the Pharmaceutical Industry 制药业感兴趣的绿色化学文章

IF 3.1 3区化学

Organic Process Research & Development Pub Date : 2024-09-10 DOI: 10.1021/acs.oprd.4c0030010.1021/acs.oprd.4c00300

Melissa A. Ashley, Miles H. Aukland, Marian C. Bryan*, Megan A. Cismesia, Theresa Dutschei, Oliver D. Engl, Pascal S. Engl, Álvaro Enriquez Garcia, Vanessa Harawa, George Karageorgis, Christopher B. Kelly, Alexandre Leclair, Johnny W. Lee, Zhen Lei, Wei Li, Jan Pawlas, Paul F. Richardson, Samuel C. Scott, Alan Steven*, Balaram S. Takale, Dauzhan Yerkozhanov and Mingshuo Zeng,

引用次数: 0

Unravelling the Impact of Process Impurities on the Crystallization of Ritlecitinib Tosylate Using Molecular Dynamics 利用分子动力学揭示工艺杂质对瑞替西替尼对甲苯磺酸盐结晶的影响

IF 3.4 3区化学

Organic Process Research & Development Pub Date : 2024-09-09 DOI: 10.1021/acs.oprd.4c00106

Clarence KeiKwan Chum, Iain Robert Gladwell, Ivan Marziano, Matteo Salvalaglio

{"title":"Unravelling the Impact of Process Impurities on the Crystallization of Ritlecitinib Tosylate Using Molecular Dynamics","authors":"Clarence KeiKwan Chum, Iain Robert Gladwell, Ivan Marziano, Matteo Salvalaglio","doi":"10.1021/acs.oprd.4c00106","DOIUrl":"https://doi.org/10.1021/acs.oprd.4c00106","url":null,"abstract":"We investigate the influence of oligomeric impurities on the crystallization of ritlecitinib tosylate, an active pharmaceutical compound, using a combined experimental and molecular modeling approach. Ritlecitinib oligomers, particularly hexamers, were identified as key species hindering crystal growth. Experimental outcomes highlighted the inhibitory effects of oligomers on crystallization kinetics, yield, and physical properties. Simplified free energy methods based on the linear interaction energy model revealed a nonmonotonic relationship between oligomer size and surface affinity, with hexamers having the most prominent tendency to block the surface of ritlecitinib tosylate crystals, thus impacting crystal growth. A competitive Langmuir adsorption isotherm model quantified the reduction in crystal growth rates due to oligomer adsorption, providing a systematic approach to understanding these inhibitory effects. This research enhances our understanding of the molecular mechanisms governing oligomer adsorption, and more generally, impurity adsorption, on crystal surfaces and offers insights for designing crystal growth inhibitors in pharmaceutical applications.","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142160906","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Catalytic Advancements: Optimizing Pd-Based Cross-Coupling Reactions Through Flow Chemistry 催化进展：通过流动化学优化钯基交叉偶联反应

IF 3.4 3区化学

Organic Process Research & Development Pub Date : 2024-09-09 DOI: 10.1021/acs.oprd.4c00027

Iqra S. Patel, Gokul Ganesan, Shilpa Jain

{"title":"Catalytic Advancements: Optimizing Pd-Based Cross-Coupling Reactions Through Flow Chemistry","authors":"Iqra S. Patel, Gokul Ganesan, Shilpa Jain","doi":"10.1021/acs.oprd.4c00027","DOIUrl":"https://doi.org/10.1021/acs.oprd.4c00027","url":null,"abstract":"Flow chemistry is a method of conducting a reaction in continuous flow through channels by pumping the reactants into the system. This advanced method offers rapid and efficient mixing, precise control of reaction conditions, high-throughput screening, and rapid optimization of the reaction as compared to batch conditions. In the current times, various pharmaceutical intermediates are being produced efficiently using flow chemistry. One of the most important reactions emerging is the carbon–carbon cross coupling reaction using transition metal catalysis especially palladium. Cross-coupling reactions are vital in the creation of advanced materials with tailored properties desired for pharmaceuticals, agrochemicals, and fine chemicals. Over the years, numerous Pd-catalyzed cross-coupling reactions, such as Suzuki-Miyaura coupling, Mizoroki-Heck coupling, Sonogashira coupling, Stille coupling, Negishi coupling, etc., have been explored and widely applied. Continuous-flow methods for heterogeneous catalysis have enhanced the reaction by integrating the separation process into a single step using packed bed reactors and eliminating the need for additional steps for catalyst recovery. The focus of this review is to address various catalysts developed for Pd-catalyzed cross-coupling reactions in a flow reaction, followed by optimization such as flow rate, residence time, temperature, Pd loading, solvent, base, and concentration of starting material. This review presents a comprehensive study of these catalysts used for C–C coupling using flow chemistry.","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142159005","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Unravelling the Impact of Process Impurities on the Crystallization of Ritlecitinib Tosylate Using Molecular Dynamics 利用分子动力学揭示工艺杂质对瑞替西替尼对甲苯磺酸盐结晶的影响

IF 3.1 3区化学

Organic Process Research & Development Pub Date : 2024-09-09 DOI: 10.1021/acs.oprd.4c0010610.1021/acs.oprd.4c00106

Clarence KeiKwan Chum, Iain Robert Gladwell, Ivan Marziano* and Matteo Salvalaglio*,

{"title":"Unravelling the Impact of Process Impurities on the Crystallization of Ritlecitinib Tosylate Using Molecular Dynamics","authors":"Clarence KeiKwan Chum, Iain Robert Gladwell, Ivan Marziano* and Matteo Salvalaglio*, ","doi":"10.1021/acs.oprd.4c0010610.1021/acs.oprd.4c00106","DOIUrl":"https://doi.org/10.1021/acs.oprd.4c00106https://doi.org/10.1021/acs.oprd.4c00106","url":null,"abstract":"We investigate the influence of oligomeric impurities on the crystallization of ritlecitinib tosylate, an active pharmaceutical compound, using a combined experimental and molecular modeling approach. Ritlecitinib oligomers, particularly hexamers, were identified as key species hindering crystal growth. Experimental outcomes highlighted the inhibitory effects of oligomers on crystallization kinetics, yield, and physical properties. Simplified free energy methods based on the linear interaction energy model revealed a nonmonotonic relationship between oligomer size and surface affinity, with hexamers having the most prominent tendency to block the surface of ritlecitinib tosylate crystals, thus impacting crystal growth. A competitive Langmuir adsorption isotherm model quantified the reduction in crystal growth rates due to oligomer adsorption, providing a systematic approach to understanding these inhibitory effects. This research enhances our understanding of the molecular mechanisms governing oligomer adsorption, and more generally, impurity adsorption, on crystal surfaces and offers insights for designing crystal growth inhibitors in pharmaceutical applications.","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":null,"pages":null},"PeriodicalIF":3.1,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.acs.org/doi/epdf/10.1021/acs.oprd.4c00106","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142270124","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Catalytic Advancements: Optimizing Pd-Based Cross-Coupling Reactions Through Flow Chemistry 催化进展：通过流动化学优化钯基交叉偶联反应

IF 3.1 3区化学

Organic Process Research & Development Pub Date : 2024-09-09 DOI: 10.1021/acs.oprd.4c0002710.1021/acs.oprd.4c00027

Iqra S. Patel, Gokul Ganesan and Shilpa Jain*,

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引用次数: 0