Journal of Flow Chemistry最新文献_第6页

A fully continuous-flow process for the synthesis of 4-nitropyrazole 用于合成 4-硝基吡唑的全连续流工艺

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-31 DOI: 10.1007/s41981-024-00311-6

Jiadi Zhou, Zhaoyang Mu, Lishan Geng, Xuyang Zhao, Chenwei Gao, Zhiqun Yu

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The continuous flow synthesis of azos 氮氧化物的连续流合成

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-26 DOI: 10.1007/s41981-024-00307-2

Adam T. McCormack, John C. Stephens

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Investigation into a high-p,T,c continuous flow synthesis of myristyl-γ-picolinium chloride (MGPC) – a preservative in pharmaceutical formulations 肉豆蔻基-γ-氯化吡啶(MGPC)的高p,T,c连续流合成研究--一种药物配方中的防腐剂

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-26 DOI: 10.1007/s41981-024-00309-0

Karuna Veeramani, Manish Shinde, Vishnuvardhana Vema Reddy Eda, Swamy Peraka, Saranya Mohan, Rakeshwar Bandichhor, Srinivas Oruganti

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Continuous flow ozonolysis of cardanol for greener synthesis of bio-based monomers 连续流臭氧分解卡丹醇，以更环保的方式合成生物基单体

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-18 DOI: 10.1007/s41981-024-00308-1

Sphurti P. Kulkarni, Amol A. Kulkarni

{"title":"Continuous flow ozonolysis of cardanol for greener synthesis of bio-based monomers","authors":"Sphurti P. Kulkarni, Amol A. Kulkarni","doi":"10.1007/s41981-024-00308-1","DOIUrl":"10.1007/s41981-024-00308-1","url":null,"abstract":"<div><p>Synthesis of bio-based monomers via continuous flow ozonolysis of cardanol using a simple tubular reactor is demonstrated. The direct ozonolysis of cardanol produces unique monomer 8-(3-hydroxyphenyl) octanal (HPOA) and heptanal along with several other oxidation products. Maximum 47% yield of HPOA with 54.3% conversion of cardanol was obtained at 0 °C in 9 s. The complete conversion of cardanol was obtained at the ozone to cardanol molar flow ratios greater than 2 at all temperatures varied in the range of -10 °C to 20 °C. Owing to large gas–liquid ratios, the mass transfer limitation for transfer of ozone from gas to liquid was negligible; however, the extent of axial dispersion in the liquid phase was significant at lower liquid flow rates. The non-ideal behavior was incorporated in the axial dispersion model to predict the conversion of cardanol. Examination of kinetic rates by both ideal plug-flow model and plug-flow with axial dispersion model revealed that the reaction is fast and is least influenced by the axial-dispersion in the reactor at prevailing operating conditions. The findings of the current study show that continuous flow technique enables a simple and safer synthesis of high-value bio-based monomers via ozonolysis of cardanol compared to traditional batch methods.</p></div>","PeriodicalId":630,"journal":{"name":"Journal of Flow Chemistry","volume":"14 2","pages":"417 - 426"},"PeriodicalIF":2.0,"publicationDate":"2024-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139495713","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

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An affordable, programmable and interactive continuous flow Photoreactor setup for undergraduate organic synthetic teaching labs 用于本科生有机合成教学实验的经济实惠、可编程和交互式连续流光反应器装置

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-18 DOI: 10.1007/s41981-023-00306-9

Michał Domański, Gilles Marcou, Joshua P. Barham

{"title":"An affordable, programmable and interactive continuous flow Photoreactor setup for undergraduate organic synthetic teaching labs","authors":"Michał Domański, Gilles Marcou, Joshua P. Barham","doi":"10.1007/s41981-023-00306-9","DOIUrl":"10.1007/s41981-023-00306-9","url":null,"abstract":"<div><p>Photochemistry and continuous flow chemistry are synthetic technology platforms that have witnessed an increasing uptake by chemical industries interested in complex organic molecule synthesis. Simultaneously, automation and data science are prominent targets in organic synthesis and in chemical industries for streamlined workflows, meaning hardware-software interaction between operators and devices is crucial. Since undergraduate teaching labs at public-funded research Universities typically (i) lack budget for commercial, user-friendly continuous flow reactors and (ii) do not teach synthetic chemists how to program or interact with reactors, there is a disparity between the skills undergraduates are equipped with and the skills that future industries need. We report a teaching lab project where undergraduates assemble, program and execute a continuous flow photoreactor to realize a multigram-scale photoredox catalyzed oxidation reaction. A palladium-free synthetic access to the starting material was described to further cut costs. Not only does this exercise introduce useful skills in reactor design, programming and wet chemistry (both photochemical and thermal, both batch and flow), it also accommodates both the typical budget and afternoon timeslot (2-3 h) of a teaching lab and can be followed by thin-layer chromatography/color changes without necessarily requiring access to NMR facilities.</p><h3>Graphical abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":630,"journal":{"name":"Journal of Flow Chemistry","volume":"14 1","pages":"349 - 355"},"PeriodicalIF":2.0,"publicationDate":"2024-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s41981-023-00306-9.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139495712","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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

Continuous flow synthesis of meso-substituted porphyrins with inline UV–Vis analysis 利用在线紫外可见光分析连续流合成介取代卟啉

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-15 DOI: 10.1007/s41981-023-00305-w

Firdaus Parveen, Henry J. Morris, Harvey West, Anna G. Slater

{"title":"Continuous flow synthesis of meso-substituted porphyrins with inline UV–Vis analysis","authors":"Firdaus Parveen, Henry J. Morris, Harvey West, Anna G. Slater","doi":"10.1007/s41981-023-00305-w","DOIUrl":"10.1007/s41981-023-00305-w","url":null,"abstract":"<div><p>Porphyrin derivatives have found diverse applications due to their attractive photophysical and catalytic properties, but remain challenging to synthesize, particularly at scale. Porphyrin synthesis thus stands to benefit from the more controlled environment, opportunities for efficient optimization, and potential for scale-up available in flow. Here, we have transferred Lindsey porphyrin synthesis into flow, enabling controlled timing for oxidation and neutralization steps and real time monitoring of the reaction mixture with inline UV–Vis analysis. For tetraphenyl porphyrin (TPP), inline UV–Vis showed the presence of protonated TPP, formed due to residual acid. Thus, inline monitoring allowed optimization of the neutralization step to improve yield. Three further porphyrin substrates were produced in flow; in two cases, the yield from inline UV was significantly higher than the yield from post-purification, identifying further yield losses that could be recovered by modifying the purification step. The workflow presented here can be adapted to multiple substrates to systematically optimise porphyrin yield, reducing the time needed to develop scalable routes to these valuable compounds.</p></div>","PeriodicalId":630,"journal":{"name":"Journal of Flow Chemistry","volume":"14 1","pages":"23 - 31"},"PeriodicalIF":2.0,"publicationDate":"2024-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s41981-023-00305-w.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139475207","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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

Solid dosing in High-Throughput Experimentation: generalization of mass enhancer technologies for submilligram scale 高通量实验中的固体配料：亚毫克级质量增强器技术的通用化

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2024-01-09 DOI: 10.1007/s41981-023-00304-x

Taline Kerackian, Géraud Chacktas, Didier Durand, Eugénie Romero

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Application of stop-flow micro-tubing reactor system in organic reaction development 停流微管反应器系统在有机反应开发中的应用

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2023-12-28 DOI: 10.1007/s41981-023-00302-z

Qian Wang, Ruize Yin, Zihan Wang, Yanbin Zhang, Jie Wu

{"title":"Application of stop-flow micro-tubing reactor system in organic reaction development","authors":"Qian Wang, Ruize Yin, Zihan Wang, Yanbin Zhang, Jie Wu","doi":"10.1007/s41981-023-00302-z","DOIUrl":"10.1007/s41981-023-00302-z","url":null,"abstract":"<div><p>Recently demonstrated as a novel reaction screening technology, the stop-flow micro-tubing (SFMT) reactors amalgamate features from continuous micro-flow and conventional batch reactors, resulting in a more logical and rigorous synthesis approach. When compared to traditional batch reactors, SFMT provides a safer and more efficient alternative, particularly suitable for chemical reactions under drastic conditions. The incorporation of commercially available transparent micro-tubing into SFMT makes it an excellent choice for light-mediated reactions, ensuring more uniform exposure to light. And SFMT stands apart from continuous-flow reactors by offering a notably convenient screening approach that is unrestricted by residence time and reactor size, while also effectively eradicating the risk of cross-contamination. The successful reactions developed within the SFMT reactor can be easily translated to continuous-flow synthesis for large-scale production. Overall, the SFMT reactor system exhibits similarities to continuous-flow reactors while surpassing batch reactors, especially for reactions involving gas reagents and/or requiring light illumination. This review aims to provide a comprehensive survey of the synthetic application of SFMT.</p></div>","PeriodicalId":630,"journal":{"name":"Journal of Flow Chemistry","volume":"14 1","pages":"97 - 107"},"PeriodicalIF":2.0,"publicationDate":"2023-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139055350","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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

Continuous synthesis of ε-caprolactone in a microreactor and kinetics insights into its side reactions 在微反应器中连续合成ε-己内酯及其副反应动力学研究

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2023-12-27 DOI: 10.1007/s41981-023-00301-0

Bin Wu, Xindi Feng, Wei Du, Zhixiang Li, Gang Qian, Xuezhi Duan, Xinggui Zhou, Zhen Liu, Jing Zhang

{"title":"Continuous synthesis of ε-caprolactone in a microreactor and kinetics insights into its side reactions","authors":"Bin Wu, Xindi Feng, Wei Du, Zhixiang Li, Gang Qian, Xuezhi Duan, Xinggui Zhou, Zhen Liu, Jing Zhang","doi":"10.1007/s41981-023-00301-0","DOIUrl":"10.1007/s41981-023-00301-0","url":null,"abstract":"<div><p>Nowadays <i>ε</i>-caprolactone, the monomer of biodegradable polycaprolactone, is mainly produced via the strong exothermic Baeyer–Villiger oxidation of cyclohexanone in semi-batch reactors. In this work, the continuous synthesis of <i>ε</i>-caprolactone was conducted in a self-designed microreactor system to address its strong exothermic feature, resulting in a cyclohexanone conversion of 90.3% and an <i>ε</i>-caprolactone yield of 82.6%. Analysis using a liquid chromatography equipped with high resolution time-of-flight mass spectrometer suggested that the byproducts mainly consist of <i>ε</i>-caprolactone oligomers in the form of dimer, trimer, and tetramer. Such oligomers were produced via hydrolysis of <i>ε</i>-caprolactone, followed by esterification of the hydrolysis product, 6-hydroxyhexanoic acid. Kinetic studies suggest that the hydrolysis reaction orders for <i>ε</i>-caprolactone and water are 0.75 and 2.52, respectively, while dimerization of 6-hydroxyhexanoic acid is a zero-order reaction. The activation energies of the hydrolysis and dimerization were ~ 77.5 kJ·mol<sup>−1</sup> and ~ 55.4 kJ·mol<sup>−1</sup>, respectively. Density functional theory calculations revealed the significant catalytic effect of acetic acid on both side reactions, where the dimerization of 6-hydroxyhexanoic acid proceeds through an alkoxy pathway.</p></div>","PeriodicalId":630,"journal":{"name":"Journal of Flow Chemistry","volume":"14 1","pages":"337 - 347"},"PeriodicalIF":2.0,"publicationDate":"2023-12-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139055245","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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

Flow chemical laboratory practice for undergraduate students: synthesis of paracetamol 本科生流程化学实验室实践：扑热息痛的合成

IF 2 4区化学

Journal of Flow Chemistry Pub Date : 2023-12-27 DOI: 10.1007/s41981-023-00303-y

Bettina Rávai, Máté János Orosz, Orsolya Péterfi, Dorián László Galata, Erika Bálint

{"title":"Flow chemical laboratory practice for undergraduate students: synthesis of paracetamol","authors":"Bettina Rávai, Máté János Orosz, Orsolya Péterfi, Dorián László Galata, Erika Bálint","doi":"10.1007/s41981-023-00303-y","DOIUrl":"10.1007/s41981-023-00303-y","url":null,"abstract":"<div><p>Generally, chemical engineering students get well acquainted with the batch synthesis of various active pharmaceutical ingredients, however, only tiny focus is provided to undergraduates on the topic of flow chemistry. In this paper, we report that students participating in the chemical engineering BSc course at the Budapest University of Technology and Economics were encouraged to perform the flow synthesis of paracetamol, a common pain painkiller. Two different synthetic routes for the continuous production of paracetamol were investigated and compared the batch and flow methods. Thus, these experiments allowed the students to discover flow chemistry for themselves under supervision: how to set up a flow system, how to carry out a reaction continuously, and to experience the advantages of flow chemistry over batch synthesis. In addition, students also got familiar with <i>in-line</i> Fourier transform infrared spectroscopy, as one of the reactions was monitored in real-time.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><img></picture></div><div><p>The educational manuscript covers the field of continuous flow synthesis of paracetamol supplemented with in-line Fourier transform infrared spectroscopy, which was developed for undergraduate students in the chemical engineering BSc course at the Budapest University of Technology and Economics</p></div></div></figure></div></div>","PeriodicalId":630,"journal":{"name":"Journal of Flow Chemistry","volume":"14 2","pages":"409 - 415"},"PeriodicalIF":2.0,"publicationDate":"2023-12-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s41981-023-00303-y.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139055234","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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