Stopped‐Flow ¹⁹ F NMR Spectroscopic Analysis of a Protodeboronation Proceeding at the Sub‐Second Time‐Scale

In-situ NMR spectroscopic analysis of homogeneous reactions is an essential tool for mechanistic in organic and organometallic chemistry. However, rapid non-equilibrium reactions, that are initiated by mixing, require specialized approaches. We report herein on a study the factors ensure quantitative results recently-developed technique stopped-flow spectroscopy. The influence some key parameters quantitation studied 19F kinetics activation base-catalyzed protodeboronation highly-reactive polyfluorinated arylboronic acids, with half-lives as low 0.1 seconds. effects spin relaxation, pre-magnetization, heat-transfer versus reaction enthalpy, mixing-efficiency analyzed detail. also compare contrast choice pulse angle, interscan delay, use pseudo real-time interleaving, means to achieve optimal balance between temporal resolution sensitivity.