High‐Throughput/High‐Output Experimentation in
            <scp>RAFT</scp>
            Polymer Synthesis

Guerrero‐Sánchez, Carlos; Yáñez‐Macías, Roberto; Rosales‐Guzmán, Miguel; Jesús‐Téllez, Marco A. De; Piñón-Balderrama, Claudia I.; Haven, Joris J.; Moad, Graeme; Junkers, Thomas; Schubert, Ulrich S.

doi:10.1002/9783527821358.ch23

Cited by 8 publications

(6 citation statements)

References 96 publications

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“…High-throughput screening in chemical synthesis improves efficiency and productivity and reduces costs. , In recent years, significant progress has been made in combining RDRP techniques with high-throughput methods, allowing rapid optimization of reaction parameters and synthesis of a diverse library of polymers with different properties . A key requirement for this combinatorial approach is improved oxygen tolerance during polymerization. , Recently, high-throughput synthesis of well-defined high molecular weight polymers via enzymatically degassed RAFT polymerization in a 96-well plate was reported .…”

Section: Introductionmentioning

confidence: 99%

Red-Light-Driven Atom Transfer Radical Polymerization for High-Throughput Polymer Synthesis in Open Air

Hu,

Szczepaniak,

Lewandowska-Andralojc

et al. 2023

J. Am. Chem. Soc.

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Photoinduced reversible-deactivation radical polymerization (photo-RDRP) techniques offer exceptional control over polymerization, providing access to well-defined polymers and hybrid materials with complex architectures. However, most photo-RDRP methods rely on UV/visible light or photoredox catalysts (PCs), which require complex multistep synthesis. Herein, we present the first example of fully oxygen-tolerant red/ NIR-light-mediated photoinduced atom transfer radical polymerization (photo-ATRP) in a high-throughput manner under biologically relevant conditions. The method uses commercially available methylene blue (MB + ) as the PC and [X−Cu II /TPMA] + (TPMA = tris(2-pyridylmethyl)amine) complex as the deactivator. The mechanistic study revealed that MB + undergoes a reductive quenching cycle in the presence of the TPMA ligand used in excess. The formed semireduced MB (MB • ) sustains polymerization by regenerating the [Cu I /TPMA] + activator and together with [X−Cu II /TPMA] + provides control over the polymerization. This dual catalytic system exhibited excellent oxygen tolerance, enabling polymerizations with high monomer conversions (>90%) in less than 60 min at low volumes (50−250 μL) and high-throughput synthesis of a library of well-defined polymers and DNA−polymer bioconjugates with narrow molecular weight distributions (Đ < 1.30) in an open-air 96-well plate. In addition, the broad absorption spectrum of MB + allowed ATRP to be triggered under UV to NIR irradiation (395−730 nm). This opens avenues for the integration of orthogonal photoinduced reactions. Finally, the MB + /Cu catalysis showed good biocompatibility during polymerization in the presence of cells, which expands the potential applications of this method.

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Section: Introductionmentioning

confidence: 99%

Red-Light-Driven Atom Transfer Radical Polymerization for High-Throughput Polymer Synthesis in Open Air

Hu,

Szczepaniak,

Lewandowska-Andralojc

et al. 2023

J. Am. Chem. Soc.

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“…Robotic high-throughput experimentation is a topic of research for many years already, both in small molecule chemistry and in polymer research. [1,2] High-throughput screening in polymer chemistry serves two purposes. First, structure-property relationships can be studied in a highly efficient way by producing and testing of polymer libraries.…”

Section: Introductionmentioning

confidence: 99%

“…Robotic high-throughput experimentation is a topic of research for many years already, both in small molecule chemistry and in polymer research. 1,2…”

Section: Introductionmentioning

confidence: 99%

Operator-independent high-throughput polymerization screening based on automated inline NMR and online SEC

et al. 2022

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“…Arguably, the most prominent such systems have come from companies such as Chemspeed Technologies and Unchained Labs, and have shown the enormous potential to enable highly complex discovery workflows across various fields in chemistry and materials science. Examples include the discovery of battery electrolytes, 13 new catalysts, [14][15][16] organic laser materials, 17,18 polymer formulations, [19][20][21] or stereoselective synthesis. 8 The current phase in the evolution of automated laboratories involves the transition from static, predefined automation workflows to modular and flexible labs where decisions about the next experimental steps are adaptively made in real time (Fig.…”

Section: Introductionmentioning

confidence: 99%

Chemspyd: An Open-Source Python Interface for Chemspeed Robotic Chemistry and Materials Platforms

Seifrid,

Strieth-Kalthoff,

Haddadnia

et al. 2024

Preprint

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We introduce Chemspyd, a lightweight, open-source Python package for operating the popular laboratory robotic platforms from Chemspeed Technologies. As an add-on to the existing proprietary software suite, Chemspyd enables dynamic communication with the automated platform, laying the foundation for its modular integration into customizable, higher-level laboratory workflows. We show the applicability of Chemspyd in a set of case studies from chemistry and materials science. We demonstrate how the package can be used with large language models to provide a natural language interface. By providing an open-source software interface for a commercial robotic platform, we hope to inspire the development of open interfaces that facilitate the flexible, adaptive integration of existing laboratory equipment into automated laboratories.

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High‐Throughput/High‐Output Experimentation in RAFT Polymer Synthesis

Cited by 8 publications

References 96 publications

Red-Light-Driven Atom Transfer Radical Polymerization for High-Throughput Polymer Synthesis in Open Air

Red-Light-Driven Atom Transfer Radical Polymerization for High-Throughput Polymer Synthesis in Open Air

Operator-independent high-throughput polymerization screening based on automated inline NMR and online SEC

Chemspyd: An Open-Source Python Interface for Chemspeed Robotic Chemistry and Materials Platforms

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