An efficient method for the NMR analysis of chiral alcohols and amines has been developed with an improved detection limit. Valentine Ananikov and Nikolay Orlov, Zelinsky Institute of Organic Chemistry, Russia, prepared samples for analysis directly in the NMR tubes; this has big advantages over existing methods to analyse these compounds.
NMR analysis of chiral compounds normally involves derivatisation with a suitable chiral agent to allow you to tell apart diastereoisomers in NMR spectra. The major limitation of this has been the fact that the derivatisation has to be done as a seperate reaction. This adds further work-up and purification procedures (generating waste), is time-consuming and means a relatively large sample is required for analysis.
However, Ananikov derivatised samples within the NMR tube, avoiding waste generation and providing samples for analysis in less than 5 min (including preparation time). All analysis could be performed on a routine NMR instrument, and could give accurate measurements for samples less than 0.01 mg. This underlines the environmentally benign and superior nature of the procedure developed by this group.
To read more, please see:
NMR analysis of chiral alcohols and amines: development of an environmentally benign “in tube” procedure with high efficiency and improved detection limit, Nikolay V. Orlov and Valentine P. Ananikov, Green Chem., 2011, DOI: 10.1039/C1GC15191F