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The resulting workflows perfectly align with approaches towards Industry 4.0 – data driven automation for development and advanced process control for manufacturing.
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9 In this context, PAT can enable faster and more reliable process optimization and enhanced process control compared to cases using offline analysis only. 8 Driven by regulatory authorities, PAT has emerged as a key tool to support pharmaceutical development, manufacturing and quality by design (QbD). The increased uptake of flow technology, particularly systems equipped with process analytical technology (PAT), 4 has opened the field to reaction optimization using advanced techniques such as design of experiments (DoE), 5 dynamic experimentation, 6 automated self-optimization 7 and feedback loops for process control. 2 Furthermore, hazardous chemistries such as highly exothermic reactions, or those involving unstable or toxic intermediates can be operated safely in flow, whereby this technology acts as a powerful route-enabler. 1 Flow technology has considerable advantages in mass- and heat transfer, safety and ease of scale-up, when compared to traditional batch reactions. Introduction In recent years continuous flow processing has attracted the interest of the fine chemical, agrochemical and pharmaceutical industries, for numerous reasons including shortened synthetic routes, improved quality and enhanced sustainability profiles. Accurate quantification of four overlapping species was possible, enabling generation of a robust DoE model along with accurate evaluation of dynamic experiments. By employing rapid data acquisition (2.0 s recording time per spectrum), we demonstrate the use of inline benchtop NMR to guide the optimization of a complex nitration reaction in flow. Using a multivariate analysis (MVA) statistical approach to data processing these hurdles can be overcome, enabling accurate quantification of complex product mixtures. Inline benchtop NMR analysis is established as a powerful tool for reaction monitoring, but its capabilities are somewhat limited by low spectral resolution, often leading to overlapping peaks and difficulties in quantification.