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

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JournalAngewandte Chemie International Edition
DateAccepted/In press - 13 Dec 2019
DateE-pub ahead of print - 9 Jan 2020
DatePublished (current) - 10 Feb 2020
Issue number7
Volume59
Number of pages5
Pages (from-to)2710-2714
Early online date9/01/20
Original languageEnglish

Abstract

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.

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