Chiral Analysis for High‐Throughput Reaction Screening: Recent Advances in Accelerating Asymmetric Catalysis Discovery

The widespread adoption of high-throughput experimentation (HTE) has transformed asymmetric catalysis by enabling the parallel execution of numerous reactions to systematically explore chemical space instead of relying on isolated trial and error. Currently, the overall efficiency of this process is limited by analytical readouts rather than reaction setups. Specifically, the rapid and reliable determination of enantiomeric excess (ee) from complex crude mixtures remains a primary bottleneck. To address this bottleneck, recent advancements in chiral analytical methodologies offer solutions through either serial analysis to shorten individual measurement times and increase information density or parallel analysis to multiplex signals for formats using microplates. These techniques span chromatography, spectroscopy, mass spectrometry, and nuclear magnetic resonance. Key factors in applying these methods include their compatibility with multiple substrates, robustness against matrix interference, and the ability to balance speed with accuracy, which allow for earlier evaluation of substrate generality and minimizes bias towards a single substrate. This proactive approach ultimately generates high-dimensional datasets that effectively guide the optimization of catalysts and reaction conditions toward universally applicable asymmetric transformations. In this review, we summarize these recent advancements in high-throughput chiral analytical methodologies and highlight their profound impact on accelerating discovery in the field of asymmetric catalysis.