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Automation and microfluidics for the efficient, fast, and focused reaction development of asymmetric hydrogenation catalysis.

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Automation and microfluidic tools potentially enable efficient, fast, and focused reaction development of complex chemistries, while minimizing resource- and material consumption. The introduction of automation-assisted workflows will contribute to the… Click to show full abstract

Automation and microfluidic tools potentially enable efficient, fast, and focused reaction development of complex chemistries, while minimizing resource- and material consumption. The introduction of automation-assisted workflows will contribute to the more sustainable development and scale-up of new and improved catalytic technologies. Herein, we describe the application of automation and microfluidics to the development of a complex asymmetric hydrogenation reaction. Screening and optimization experiments were performed using an automated microfluidic platform, which enabled a drastic reduction in the material consumption compared to conventional laboratory practices. A suitable catalytic system was identified from a library of Ru II -diamino precatalysts. In situ precatalyst activation was studied with 1 H/ 31 P NMR, and the reaction was scaled up to multigram quantities in a batch autoclave. These reactions were monitored using an automated liquid-phase sampling system. Ultimately, our automation-assisted approach provided multigram quantities of the target enantiopure alcohol product in less than a week of total experimental time.

Keywords: automation; development; fast focused; efficient fast; reaction; focused reaction

Journal Title: ChemSusChem
Year Published: 2022

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