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Published on: January 4, 2018
Automation and Microfluidics for the Efficient, Fast, and Focused Reaction Development of Asymmetric Hydrogenation
Robbert van Putten1,2, Natalie S Eyke2, Lorenz M Baumgartner2
1Inorganic Systems Engineering, Department of Chemical Engineering, Delft University of Technology, Van der Maasweg 9, 2629HZ, Delft, Netherlands.
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, the application of automation and microfluidics to the development of a complex asymmetric hydrogenation reaction is described. 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 RuII -diamino precatalysts. In situ precatalyst activation was studied with 1 H/31 P nuclear magnetic resonance (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, in less than a week of total experimental time, multigram quantities of the target enantiopure alcohol product were provided by this automation-assisted approach.
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