Real-Time Analysis for Quality Control of a Reaction Process using Ultra-high Performance Liquid Chromatography. Reduction of Phenyl Ketone to Phenyl Alcohol

The applicability of ultra-high performance liquid chromatography (UHPLC) for real-time analysis of a synthetic process was examined. A reduction reaction was selected as a model process. Quantities of acetophenone (AcPh) and phenyl ethanol (PhEt) in reaction solutions were analyzed at 5- and 15-min intervals. Reaction solutions were diluted using acetonitrile and subsequently filtered. A mixture of acetonitrile and water (6:4) was used as the mobile phase. PhEt and AcPh were detected at 0.64 and 0.75 min, respectively. Additionally, as many as nine different impurities were detected in the reaction solution. Given the ability to detect impurities in a reaction solution within a few minutes, UHPLC technology is deemed applicable for real-time synthetic process control.