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

TY - JOUR

T1 - The Detection and Reactivity of Silanols and Silanes Using Hyperpolarized 29Si Nuclear Magnetic Resonance

AU - Duckett, Simon B.

AU - Rayner, Peter John

AU - Richardson, Peter Michael

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PY - 2020/2/10

Y1 - 2020/2/10

N2 - Silanols and silanes are key precursors and intermediates for the synthesis of silicon-based materials. While their characterization and quantification using 29Si NMR 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 are 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.

AB - Silanols and silanes are key precursors and intermediates for the synthesis of silicon-based materials. While their characterization and quantification using 29Si NMR 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 are 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.

U2 - 10.1002/anie.201915098

DO - 10.1002/anie.201915098

M3 - Article

SN - 1433-7851

VL - 59

SP - 2710

EP - 2714

JO - Angewandte Chemie International Edition

JF - Angewandte Chemie International Edition

IS - 7

M1 - 201915098

ER -