Integration of enabling methods for the automated flow preparation of piperazine-2-carboxamide

Ingham, Richard J.; Battilocchio, Claudio; Hawkins, Joel M.; Ley, Steven V.

doi:10.3762/bjoc.10.56

Cited by 73 publications

(71 citation statements)

References 27 publications

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“…A similar approach has been followed in most systems reported to date, in which self-optimization has been implemented. These systems cover different areas of chemistry: polymerization reaction [13 ,14 ], heterogeneous catalytic processes [1,2,5], droplet formation [15,16] assembly of nanoparticles [17] and even multi-step syntheses [4,[18][19][20][21]. As we shall show below, this approach to automation is readily extendable to include chemoinformatics and design of experiments, using data exchange standards, such as OPC.…”

Section: Hardware For Self-optimization Of Closed-loop Systems Labwarementioning

confidence: 98%

Automatic discovery and optimization of chemical processes

Houben

Lapkin

2015

Current Opinion in Chemical Engineering

105

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This paper presents the first overview of recent developments in techniques and methods that enable closed-loop optimization, also sometimes called 'self optimization', as well as discovery in different areas of molecular sciences. The closed-loop experimental platforms offer tremendous new opportunities by significantly increasing productivity, as well as enabling completely new types of experiments to be performed. Such experiments involve three main enabling technology areas: automated experimental systems, analytical instruments connected to automated chemoinformatics software and optimization or decision-making algorithms. We review the most exciting developments concerning robotic experiments, 3D printed lab-ware, experimental systems with multiple analytical instruments and advanced optimization algorithms based on machine learning approaches. A range of different chemical problems is described, which show the breadth of potential applications of this emerging experimental approach.

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Section: Hardware For Self-optimization Of Closed-loop Systems Labwarementioning

confidence: 98%

Automatic discovery and optimization of chemical processes

Houben

Lapkin

2015

Current Opinion in Chemical Engineering

105

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“…For instance, in the system for automated synthesis of piperazine-2-carboxamide, a component of a drug for the treatment of tuberculosis, a flow FTIR detector was employed, together with continuous monitoring of the level of liquid in reservoir, using digital camera, and a plastic float in reservoir [95]. In another automated system for multi-step synthesis of pyrazole, two in-line FTIR monitors were applied to control additional pumps to dispense reagents following the unavoidable dispersion on the reaction segment (Fig.12A) [96].…”

Section: Analytical Monitoring In Continuous Flow Synthetic Systemsmentioning

confidence: 99%

Flow chemistry vs. flow analysis

Trojanowicz

2016

Talanta

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“…In 2014, Ley group illustrated the use of an open-source software package integrated with a laboratory hardware to develop and optimize a machine-assisted flow synthesis of pyperazine-2-carboxamide (51), a component of the antituberculosis Rifater (Scheme 15) [34]. The reaction consisted in the hydration of nitrile 52 to amide 53 followed by a hydrogenation step.…”

Section: Central Composite Designmentioning

confidence: 99%

Concepts and Optimization Strategies of Experimental Design in Continuous-Flow Processing

Gioiello¹,

Filipponi²,

Mostarda³

et al. 2016

J Flow Chem

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The integration of flow systems with statistical design of experiments is emerging as a valuable strategy to develop new synthetic routes towards relevant building blocks, chemical probes, and drug compounds. Optimization by experimental design incorporates statistical algorithms, mathematical models and equations, predicting tools, feedback control, and validation to generate new optimal conditions. Continuous-flow chemistry is ideally suited for this scope, as the integration of in-line analysis is simple; experimental parameters such as temperature, pressure, and flow rate can be easily controlled and fine-regulated; and automation of reaction screening can be accomplished with software assistance. This review article aims to illustrate how the combination of flow synthesizers and design of experiments can be profitable to speed up the development and optimization of more efficient, safer, and reproducible protocols for modern synthetic methods and manufacturing processes.

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Integration of enabling methods for the automated flow preparation of piperazine-2-carboxamide

Cited by 73 publications

References 27 publications

Automatic discovery and optimization of chemical processes

Automatic discovery and optimization of chemical processes

Flow chemistry vs. flow analysis

Concepts and Optimization Strategies of Experimental Design in Continuous-Flow Processing

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