Optimizing processes is an integral part of chemical research and development. The attractiveness of any chemical reaction depends on the yield and quality of the desired product, the time required for conversion, the process cost and many other factors. This is true for academic environments as well as industrial research and development in the chemical and pharmaceutical industry. E.g. Design of Experiments (DoE) or retrosynthetic algorithms are commonly applied to identify the most attractive reaction conditions. However, the traditionally manual execution of the associated experiments including data acquisition and processing is time-consuming, prone to human error, and often lacks reproducibility.

Chemspeed’s automated synthesis and process research workstations offer a sophisticated operator-independent and reproducible way to setup parallel experiments testing the variables defined in the DoE simultaneously. As the workflow does not require user intervention after the setup, the experimentation can be continuously performed beyond the working hours of the scientists or laboratory technicians. The cutting-edge synthesis and process research workstation technology allows scientists to execute and perform a variety of workflows (reaction preparation, reaction execution, work-up, analysis) in a fully automated fashion and truly mimic the final industrial production process. It provides all the flexibility to optimize integrated reaction sequences, even if a complex configuration of reactors and feed vessels is required.

NMR spectroscopy is key for the evaluation of any reactions performance as it allows for identification and quantification of starting materials, reactants, products and any by-products formed. Therefore, combining Chemspeed’s automation workstations with the cryogen-free benchtop NMR spectrometer Fourier 80 and utilizing Bruker’s Advanced Chemical Profiling software for automated NMR data processing, a one-stop-shop for chemical process optimization is formed.

High-level workflow:

1. Chemspeed’s Screening workstation executes parallelized transesterification reactions in a fully automated workflow. Similarly, coupling reactions (such as Suzuki, Buchwald, Heck, etc.) could be executed in an analogous workflow.

2. At designated intervals, the platform prepares an aliquot for analysis and the Bruker Fourier 80 benchtop NMR Spectrometer acquires the data.

3. Bruker’s Advanced Chemical Profiling (ACP) analyzes and processes the data.

4. Chemspeed’s AutoSuite software can then utilize the data feedback to adjust/optimize reaction parameters.