Safety aspects of Grignard reactions are well documented; and PAT (Process Analytical Technology) has been utilized extensively for industrial processing. The presentation reports lab and pilot plant development efforts with a line of sight to manufacturing installation. Results using the Attenuated Total Reflection Fourier Transform Infrared (ATR-FTIR), NIR, and Raman spectroscopy are described along with the challenges encountered with each technology during scale-up. Additionally, the effect of particle size, mixing, and magnesium grade on reaction kinetics were measured on both the laboratry- and pilot plant scale.