Bell, N. L. , Boser, F., Bubliauskas, A., Willcox, D. R., Sandoval Luna, V. E. and Cronin, L. (2024) Autonomous execution of highly reactive chemical transformations in the Schlenkputer. Nature Chemical Engineering, 1, pp. 180-189. (doi: 10.1038/s44286-023-00024-y)
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Abstract
We design a modular programmable inert-atmosphere Schlenkputer (Schlenk-line computer) for the synthesis and manipulation of highly reactive compounds, including those that are air and moisture sensitive or pyrophoric. Here, to do this, we constructed a programmable Schlenk line using the Chemputer architecture for the inertization of glassware that can achieve a vacuum line pressure of 1.5 × 10−3 mbar, and integrated a range of automated Schlenk glassware for the handling, storage and isolation of reactive compounds at sub-ppm levels of O2 and H2O. This has enabled automation of a range of common organometallic reaction types for the synthesis of four highly reactive compounds: [Cp2TiIII(MeCN)2]+, CeIII{N(SiMe3)2}3, B(C6F5)3 and {DippNacNacMgI}2, which are variously sensitive to temperature, pressure, water and oxygen. Automated crystallization, filtration and sublimation are demonstrated, along with analysis using inline nuclear magnetic resonance or reaction sampling for ultraviolet–visible spectroscopy. Finally, we demonstrate low-temperature reactivity down to −90 °C as well as safe handling and quenching of alkali metal reagents using dynamic feedback from an in situ temperature probe.
| Item Type: | Articles |
|---|---|
| Additional Information: | Financial support from the Engineering and Physical Sciences Research Council (grant nos. EP/L023652/1, EP/R020914/1, EP/S030603/1, EP/R01308X/1, EP/S017046/1 and EP/S019472/1), the European Research Council (project no. 670467 SMART-POM), the European Commission (project no. 766975 MADONNA) and Defense Advanced Research Projects Agency (project nos. W911NF-18- 2-0036, W911NF-17-1-0316 and HR001119S0003). |
| Status: | Published |
| Refereed: | Yes |
| Glasgow Author(s) Enlighten ID: | Boser, Florian and Sandoval Luna, Victor Esteban and Willcox, Dr Dominic and Bell, Dr Nicola and Cronin, Professor Lee and Bubliauskas, Andrius |
| Authors: | Bell, N. L., Boser, F., Bubliauskas, A., Willcox, D. R., Sandoval Luna, V. E., and Cronin, L. |
| College/School: | College of Science and Engineering > School of Chemistry |
| Journal Name: | Nature Chemical Engineering |
| Publisher: | Nature Research |
| ISSN: | 2948-1198 |
| ISSN (Online): | 2948-1198 |
| Copyright Holders: | Copyright © The Author(s) 2024 |
| First Published: | First published in Nature Chemical Engineering 1:180-189 |
| Publisher Policy: | Reproduced under a Creative Commons license |
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