Abstract
Real-time NMR spectroscopy has proven to be a rapid and an effective monitoring tool to study the hypervalent iodine(III) mediated cyclopropanation. With the ever increasing number of new synthetic methods for carbon–carbon bond formation, the NMR in situ monitoring of reactions is becoming a highly desirable enabling method. In this study, we have demonstrated the versatility of benchtop NMR using inline and online real-time monitoring methods to access mutually complementary information for process understanding, and we developed new approaches for real-time monitoring addressing challenges associated with better integration into continuous processes.
Highlights
The understanding, quality, and control of chemical processes are of vital importance from early discovery through to process optimization and scale-up onto full scale manufacturing
In conclusion we have reported the efficient use of state-of-theart benchtop nuclear magnetic resonance (NMR) technology for online monitoring of reaction progress over time, and inline tracking of the steadystate of continuous flow processes
Despite the lower field of the reported benchtop NMR, surprisingly useful information arises as a result of the high-homogeneity permanent magnet design, and the efficient reaction monitoring hardware and software interface
Summary
The understanding, quality, and control of chemical processes are of vital importance from early discovery through to process optimization and scale-up onto full scale manufacturing. Organic Process Research & Development the cyclopropanation progress acquired using the 1H NMR data from the nine spectra array clearly demonstrated the progression of the ethyl group on product 5 (δH 0.5−1.1) in parallel to the disappearance of the acetate ligands of DIB, the methylene moiety of α-nitroacetate 4 and the geminal protons of styrene 2 (Figure 7b). DIB reagents or by enhancing solubility with ring functionalization such as o-alkoxyphenyliodonium derivatives.[21] A similar balance is found with reaction temperature which, while generally favoring reactivity, can create polymerization of some styrene substrates at higher temperatures especially when bearing an electron withdrawing group These preliminary studies generally demonstrate the potential of the hypervalent iodine(III) mediated cyclopropanation continuous process
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