Deprotection of <i>N</i>-Boc Groups under Continuous-Flow High-Temperature Conditions

Bryan Li, Ruizhi Li, Peter H. Dorff, J. Christopher McWilliams, Robert M. Guinn, Steven M. Guinness, Lu Han, Ke Wang, Shu Yu

The Journal of Organic Chemistry · 2019 · 47 citations · 34 references

Concepts

Abstract

The scope of thermolytic, N-Boc deprotection was studied on 26 compounds from the Pfizer compound library, representing a diverse set of structural moieties. Among these compounds, 12 substrates resulted in clean (≥95% product) deprotection, and an additional three compounds gave ≥90% product. The thermal de-Boc conditions were found to be compatible with a large number of functional groups. A combination of computational modeling, statistical analysis, and kinetic model fitting was used to support an initial, slow, and concerted proton transfer with release of isobutylene, followed by a rapid decarboxylation. A strong correlation was found to exist between the electrophilicity of the N-Boc carbonyl group and the reaction rate.

References

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