Solid-state reactions using mechanochemical activation have emerged as solvent-free atom-efficient strategies for sustainable chemistry. Herein we report a new mechanochemical approach for the amide
Spin-spin coupling constants between nuclei in NMR spectroscopy reflect their spatial arrangement. A number of calculation methods, applying different levels of theory, have been developed to support the stereochemical assignment of novel compounds. Nevertheless, revisions of the assignment of structures in the literature are not rare. In the present work, the reliability of the calculation methods amenable for a theoretical prediction of spin-spin coupling constants of vicinal protons to support correct stereochemical assignment of substitution at five-membered rings of 3-alkoxy-6,7-epoxy-2-oxabicyclo[3.3.0]octanes was studied. Experimental (3)J(H,H) coupling constants were compared with the coupling constants calculated for all possible diastereomers. The fully quantum chemical approach provided theoretical (3)J(H,H) coupling constants with an absolute deviation of no more than 1.1 Hz for 91% of the experimentally studied coupled spins, whereas the methods without quantum chemical geometry optimization resulted in completely unreliable predictions. Consequently, for a reliable stereochemical assignment of small and medium size molecules, the protocol for calculating the coupling constants based on the results of the quantum chemical geometry optimization is recommended.
Methylphosphonic acid (MPA) is introduced as an internal standard for the determination of the phosphorus content of carbonated beverages (cola drinks) by quantitative 31 P-NMR analysis.Phosphorus in cola beverages was analyzed as phosphate in ten commercially available drinks.Phosphate concentration in the studied samples was in the range of 3.5 to 6.1 mM. The preparation of the samples included: degassing of commercially available beverages, addition of MPA as an internal standard, D 2 O for signal locking and a solution of NaOH to ensure a basic environment in the sample. The calibration graphs of the MPA standard and analyte showed a linear response in the concentration range of interest. The measured values of the phosphoric acid standard solutions lay within the confidence limits of the MPA, showing that these compounds give a similar response in NMR analysis. The measured concentrations of phosphorus were in good agreement with the values detected by the traditional spectrophotometric method. The presented 31 P-NMR method using MPA as an internal standard is reliable and simple for the determination of the phosphorus content of cola type beverages.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.