IN-SITU FOURIER-TRANSFORM INFRARED AND CALORIMETRIC STUDIES OF THE PREPARATION OF A PHARMACEUTICAL INTERMEDIATE

Utilizing in-situ Fourier transform infrared (FT-IR) spectroscopy coup led with an automated laboratory reaction calorimeter, a complex and p otentially energetic reaction was investigated in a continuously stirr ed tank reactor (CSTR) system. The FT-IR data has led to mechanistic i nsight and the development of a rapid compositional monitor. This capa bility leads to high quality kinetic data. Additionally, the detail in the FT-IR data allows for statistical tests which may alert investiga tors of deviations from desired operating conditions. The calorimeter provided the components required to elucidate a material and energy ba lance for all streams, thus contributing to the reaction system design for factory-scale operation. This study demonstrates the utility of c oupling automated laboratory reaction systems with on-line analysis fo r both basic research and process development objectives.