(488c) Enhanced Development and Control of Continuous Processes Using Real Time in Situ FTIR Analytics

Multiple reactions were studied using ATR-FTIR as a convenient, specific, inline monitoring technique to examine various aspects, challenges, and opportunities posed by flow chemistry: Dispersion in the column, rapid screening of reaction conditions, reactive intermediate identification, hazardous compound detection to protect the experimenter, microliter scales experiments. This initial study showed that the time it usually takes to optimize reaction conditions was shortened Due to the fast response time and  structural information in each of the many reaction mixture spectra obtained, short-lived intermediates were observed in situ, which helped gain a better understanding of reaction mechanism. In a later investigation, formation of a pyrazole derivative, the use of ATR-FTIR enabled precise control of reagent streams addition in a complex multi-step reactions sequence. For the first time, it is therefore possible to control pumps to dispense reagents based upon the real time concentration of reaction intermediates in multi-step processes. As a result of this high level of control via inline monitoring, multi-step sequences were run more efficiently. For instance, in the event of a reaction failure, precious material would be saved since the lowered concentration of intermediate would be accounted for in real-time.