959044-31-6Relevant articles and documents
Titration of nonstabilized diazoalkane solutions by fluorine NMR
Rendina, Victor L.,Kingsbury, Jason S.
experimental part, p. 1181 - 1185 (2012/03/12)
A new protocol for titrating nonstabilized diazoalkane solutions by quantitative 19F NMR is reported. An excess of 2-fluorobenzoic acid dissolved in CDCl3 is treated with the diazoalkane solution at a low temperature, immediately forming the corresponding 2-fluorobenzoate ester upon warming. A significant difference in the 19F chemical shift between the ester and acid is seen, allowing facile and accurate integration to determine titer. The procedure is safe, rapid, and indicates the active diazoalkane concentration with high precision.