Residual Solvent Signal of CDCl3 as a qNMR Internal Standard for Application in Organic Chemistry Laboratory
Journal of Organic Chemistry 2021
R Muhamadejev, Renāte Melngaile, P Paegle, I Zibarte, M Petrova, K Jaudzems, Jānis Veliks

A nuclear magnetic resonance (NMR) spectrometer is a key instrument in the organic synthesis laboratory for structure determination, reaction control, and compound purity analysis. In addition to qualitative analysis, the application of NMR for quantitative analysis (qNMR) is gaining popularity. qNMR allows for simple quantification of crude product mixtures, determination of reaction yields, and purity of organic compounds. The determination of NMR yield requires the addition of an internal standard to each sample. Herein, we report a method where CDCl3 residual solvent signal is used as an internal standard for qNMR after quantification in the solvent batch. This method significantly simplifies sample preparation and allows straightforward recovery of the analyte by the simple evaporation of the NMR solvent. The accuracy of the method is comparable to qNMR with 1,3,5-trimethoxybenzene as an internal standard if the herein described guidelines are followed.


Keywords
Internal standards; Organic chemistry laboratory; Organic synthesis; Qualitative analysis; Reaction control; Residual solvents; Sample preparation; Structure determination
DOI
10.1021/acs.joc.0c02744
Hyperlink
https://pubs.acs.org/doi/10.1021/acs.joc.0c02744

Muhamadejev, R., Melngaile, R., Paegle, P., Zibarte, I., Petrova, M., Jaudzems, K., Veliks, J. Residual Solvent Signal of CDCl3 as a qNMR Internal Standard for Application in Organic Chemistry Laboratory. Journal of Organic Chemistry, 2021, Vol. 86, No. 5, pp.3890-3896. ISSN 0022-3263. e-ISSN 1520-6904. Available from: doi:10.1021/acs.joc.0c02744

Publication language
English (en)
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