The Detection and Reactivity of Silanols and Silanes Using Hyperpolarized 29Si Nuclear Magnetic Resonance

Silanols and silanes are key precursors and intermediates for the synthesis of silicon‐based materials. While their characterization and quantification by ²⁹Si NMR spectroscopy has received significant attention, it is a technique that is limited by the low natural abundance of ²⁹Si and its low sensitivity. Here, we describe a method using p‐H₂ to hyperpolarize ²⁹Si. The observed signal enhancements, approaching 3000‐fold at 11.7 T, would take many days of measurement for comparable results under Boltzmann conditions. The resulting signals were exploited to monitor the rapid reaction of tris(tert‐butoxy)silanol with triflic anhydride in a T₁‐corrected process that allows for rapid quantification. These results demonstrate a novel route to quantify dynamic processes and intermediates in the synthesis of silicon materials.