Rapid identification of the short-lived intermediates in alternating-current electrolysis by mass spectrometry

Abstract

Herein, we report the rapid mass spectrometric identification of the short-lived intermediates generated under AC electrolysis via combining bipolar electrochemistry with nanoelectrospray ionization in a hybrid ultramicroelectrode/ion emitter. The key reactive intermediates involved in the C–O/O–H cross-metathesis between 4-alkoxy anilines and alcohols were successfully captured and identified for the first time, providing direct evidence for the previously proposed mechanism.