Autonomous Execution of Highly Reactive Chemical Transformations in the Schlenkputer

We demonstrate how it is possible to design a modular programmable inert-atmosphere Schlenkputer (Schlenk-line-computer) for the synthesis and manipulation of the most highly reactive compounds including those which are air- and moisture sensitive or pyrophoric. To do this we have designed and built a programmable Schlenk Line using the Chemputer architecture for the inertization of glassware which 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. Utilising this hardware in conjunction with our platform has allowed the automation of a range of common organometallic reaction types for the synthesis of four highly reactive compounds from across the periodic table: [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 purification by crystallisation, filtration and sublimation are each demonstrated along with analysis using inline NMR or reaction sampling for UV/Vis. Finally, we demonstrate automated ultra-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.