Thermoresponsive Alignment Media in NMR Spectroscopy: Helix Reversal of a Copolyaspartate at Ambient Temperatures

Chemistry : a European Journal
Mira SchwabChristina M Thiele

Abstract

Poly(aspartic acid esters) are known to form either right-or left-handed α-helices depending on the ester group in the side chain, on solvent and/or on temperature. Polyphenethyl-l-aspartates (PPLA) exhibit a helix reversal from the right- to the left-handed form with increasing temperature. We have recently reported the application of polyphenethylaspartates as helically chiral alignment media. The thermoresponsivity observed for these polymers offers the possibility to measure different orientations of analytes before and after helix reversal of the alignment medium at 373 K. Herein we present a synthesized copolymer of phenethyl- and benzylaspartate as a new alignment medium undergoing this helix reversal at 303-313 K. Thus, the measurement of residual dipolar couplings (RDC) before and after the helix reversal is allowed for at ambient temperatures. A complete sign change of all 1 H-13 C RDCs was observed, which is close to the highest possible difference in NMR spectra.

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Citations

Jul 11, 2019·Magnetic Resonance in Chemistry : MRC·Anna DopplerMichael John
Jun 11, 2020·Chemical Communications : Chem Comm·Ikenna E NdukweR Thomas Williamson
Mar 5, 2020·Progress in Nuclear Magnetic Resonance Spectroscopy·Philippe LesotOlivier Lafon
Oct 23, 2021·The Journal of Organic Chemistry·Felix A RothChristina M Thiele
Dec 10, 2021·Physical Chemistry Chemical Physics : PCCP·Felix A RothChristina M Thiele

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