A Quantitative NMR Method for Silyllithium AnalysisThis work was supported by the National Institute of General Medical Sciences (grant number R01GM076471).
Received: 14 August 2017
Accepted after revision: 17 August 2017
05 September 2017 (eFirst)
Published as part of the Cluster Silicon in Synthesis and Catalysis
A rapid and extremely simple method for silyl anion analysis is presented. The progress of silyllithium reagent preparation can be determined by quenching an aliquot with neat chloro(trimethyl)silane, evaporation, dilution with CDCl3, and direct proton NMR analysis. This procedure is fast, simple, and allows for identification and relative quantification of the starting reagent, intermediates, and the silyllithium product.