One Sentence Summary: A modular platform for synthesis is demonstrated that makes purified organic compounds autonomously without physical reconfiguration and is driven using a chemical programming language.Abstract: The synthesis of complex organic compounds is largely a manual process that is often incompletely documented. To address these shortcomings, we developed an abstraction that maps commonly reported methodological instructions into discrete steps amenable to automation. These unit operations were implemented in a modular robotic platform using a chemical programming language which formalizes and controls the assembly of the molecules.We validated the concept by directing the automated system to synthesize three pharmaceutical compounds, Nytol, Rufinamide, and Sildenafil, without any human intervention. Yields and purities of products and intermediates were comparable to or better than those achieved manually. The syntheses are captured as digital code that can be published, versioned, and transferred flexibly between platforms with no modification, thereby greatly enhancing reproducibility and reliable access to complex molecules.The automation of chemical synthesis is currently expanding, and this is driven by the availability of digital labware. The field currently encompasses areas as diverse as the design of new reactions (1), chemistry in reactionware (2), reaction monitoring and optimization (3,4), flow chemistry (5) for reaction optimization and scale up, to full automation of the synthesis
In recent decades, 3D printing (also known as additive manufacturing) techniques have moved beyond their traditional applications in the fields of industrial manufacturing and prototyping to increasingly find roles in scientific research contexts, such as synthetic chemistry. We present a general approach for the production of bespoke chemical reactors, termed reactionware, using two different approaches to extrusion-based 3D printing. This protocol describes the printing of an inert polypropylene (PP) architecture with the concurrent printing of soft material catalyst composites, using two different 3D printer setups. The steps of the PROCEDURE describe the design and preparation of a 3D digital model of the desired reactionware device and the preparation of this model for use with fused deposition modeling (FDM) type 3D printers. The protocol then further describes the preparation of composite catalyst-silicone materials for incorporation into the 3D-printed device and the steps required to fabricate a reactionware device. This combined approach allows versatility in the design and use of reactionware based on the specific needs of the experimental user. To illustrate this, we present a detailed procedure for the production of one such reactionware device that will result in the production of a sealed reactor capable of effecting a multistep organic synthesis. Depending on the design time of the 3D model, and including time for curing and drying of materials, this procedure can be completed in ∼3 d.
Electrodes from the ink‐jet printer: Cellulose sheets can be transformed into mesostructured graphene nanostructures by a simple and general method. Since the iron catalyst can be printed on paper with an ink‐jet printer, the products can be prepared with 2D patterns. Subsequent Cu deposition results in further functionalization of the microstructured electrodes (see picture).
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