RAPID INJECTION NMR: A SIMPLE TECHNIQUE FOR THE OBSERVATION OF REACTIVE INTERMEDIATES

Article abstract of DOI:10.1002/mrc.1270170114

A system has been designed for the NMR observation (at 60 MHz) of unstable intermediates, with half-lives of 100 ms, at concentration levels above 1E-2 M.Rapid mixing can be achieved in less than 40 ms and a series of eight spectra acquired in less than 1.08 s.Low temperature operation is straightforward.Reactive intermediates involved in the reaction of methylamine with 2,4,6-trinitroanisole and the acid-catalysed hydrolysis of 1,1-diethoxy-2,3-diphenylcycloprop-2-ene were identified, and in a kinetic application, the rate of hydrolysis of trimethyloxonium tetrafluoroborate was measured.