Selective separation of amines from continuous processes using automated pH controlled extraction

Power, Luke A.; Clayton, Adam D.; Reynolds, William R.; Hose, David R. J.; Ainsworth, Caroline; Chamberlain, Thomas W.; Nguyen, Bao; Bourne, Richard A.; Kapur, Nikil; Blacker, A. John

doi:10.1039/d1re00205h

Cited by 5 publications

(8 citation statements)

References 26 publications

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“…To purify a mixture by tuning its pH, the target compound must be ionizable. Recently, Blacker and co-workers developed an autonomous system for screening liquid-liquid extraction conditions using a Zaiput membrane [53]. The system is monitored by both online and inline analysis to control the acid concentration.…”

Section: Inline Extractions/separationsmentioning

confidence: 99%

Inline purification in continuous flow synthesis – opportunities and challenges

García-Lacuna¹,

Baumann²

2022

Beilstein J. Org. Chem.

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Continuous flow technology has become the method of choice for many academic and industrial researchers when developing new routes to chemical compounds of interest. With this technology maturing over the last decades, robust and oftentimes automated processes are now commonly exploited to generate fine chemical building blocks. The integration of effective inline analysis and purification tools is thereby frequently exploited to achieve effective and reliable flow processes. This perspective article summarizes recent applications of different inline purification techniques such as chromatography, extractions, and crystallization from academic and industrial laboratories. A discussion of the advantages and drawbacks of these tools is provided as a guide to aid researchers in selecting the most appropriate approach for future applications. It is hoped that this perspective contributes to new developments in this field in the context of process and cost efficiency, sustainability and industrial uptake of new flow chemistry tools developed in academia.

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Section: Inline Extractions/separationsmentioning

confidence: 99%

Inline purification in continuous flow synthesis – opportunities and challenges

García-Lacuna¹,

Baumann²

2022

Beilstein J. Org. Chem.

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“…8−10 One purification step that has attracted significant attention in the flow chemistry community is the extraction of products or impurities based on their partitioning between immiscible liquids. 5,11,12 Liquid−liquid extraction brings benefits including: (i) operation at low temperatures and pressures, of importance when heat sensitive materials require processing; 13 (ii) high selectivity when combining multiple stages, ideal when components are present in small quantities and require recovery or removal; 14 and (iii) the ease of use of green and renewable solvents such as those derived from biomaterials which are generally less volatile than crude oil based solvents which are therefore separated more readily by differences in their solubilities rather than by distillation. 15,16 Several laboratory scale devices have been designed to separate immiscible liquids in order to facilitate liquid−liquid extraction processes.…”

Section: ■ Introductionmentioning

confidence: 99%

A Coalescing Filter for Liquid–Liquid Separation and Multistage Extraction in Continuous-Flow Chemistry

Daglish,

Blacker,

de Boer

et al. 2024

Org. Process Res. Dev.

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Presented here is the design and performance of a coalescing liquid−liquid filter, based on low-cost and readily available meltblown nonwoven substrates for separation of immiscible phases. The performance of the coalescer was determined across three broad classes of fluid mixtures: (i) immiscible organic/aqueous systems, (ii) a surfactant laden organic/aqueous system with modification of the type of emulsion and interfacial surface tension through the addition of sodium chloride, and (iii) a water− acetone/toluene system. The first two classes demonstrated good performance of the equipment in effecting separation, including the separation of a complex emulsion system for which a membrane separator, operating through transport of a preferentially wetting fluid through the membrane, failed entirely. The third system was used to demonstrate the performance of the separator within a multistage liquid−liquid counterflow extraction system. The performance, robust nature, and scalability of coalescing filters should mean that this approach is routinely considered for liquid−liquid separations and extractions within the fine chemical and pharmaceutical industry.

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“…[13][14][15] Continuous-flow processes within the fine chemicals sector are being widely explored and have shown benefits in reaction selectivity and yield. 16 Microreactor technology has increased interest in the synthesis of a variety of organic molecules and medicinal drugs. 17 In pharmaceutical drug development production costs and time can be reduced with the use of continuous-flow technologies.…”

Section: Introductionmentioning

confidence: 99%

Magnetically agitated continuous-flow tube reactors with aspartate ammonia-lyase immobilized on magnetic nanoparticles

et al. 2023

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Selective separation of amines from continuous processes using automated pH controlled extraction

Abstract: We present a rapid continuous processing methodology to screen for the optimal, selective, liquid-liquid extraction conditions, from a typical post-reaction mixture of amines, using both inline and online analysis to...

Cited by 5 publications

References 26 publications

Inline purification in continuous flow synthesis – opportunities and challenges

Inline purification in continuous flow synthesis – opportunities and challenges

A Coalescing Filter for Liquid–Liquid Separation and Multistage Extraction in Continuous-Flow Chemistry

Magnetically agitated continuous-flow tube reactors with aspartate ammonia-lyase immobilized on magnetic nanoparticles

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