Controlled interconversion of macrocyclic atropisomers via defined intermediates.

Sun, Xin; Bai, Jin-Ku; Yang, Yu-Dong; Zhu, Ke-Lin; Liang, Jia-Qi; Wang, Xin-Yue; Xiang, Jun-Feng; Hao, Xiang et al. · Nat Commun · 2024

basic_science · Level V

Where this comes from

Abstract

Macrocyclic conformations play a crucial role in regulating their properties. Our understanding of the determinants to control macrocyclic conformation interconversion is still in its infancy. Here we present a macrocycle, octamethyl cyclo[4](1,3-(4,6)-dimethylbenzene)[4]((4,6-benzene)(1,3-dicarboxylate) (OC-4), that can exist at 298 K as two stable atropisomers with C<sub>2v</sub> and C<sub>4v</sub> symmetry denoted as C<sub>2v</sub>-OC-4 and C<sub>4v</sub>-OC-4, respectively. Heating induces the efficient stepwise conversion of C<sub>2v</sub>- to C<sub>4v</sub>-OC-4 via a C<sub>s</sub>-symmetric intermediate (C<sub>s</sub>-OC-4). It differs from the typical transition state-mediated processes of simple C-C single bond rotations. Hydrolysis and further esterification with a countercation dependence promote the generation of C<sub>2v</sub>- and C<sub>s</sub>-OC-4 from C<sub>4v</sub>-OC-4. In contrast to C<sub>2v</sub>-OC-4, C<sub>4v</sub>-OC-4 can bind linear guests to form pseudo-rotaxans, or bind C<sub>60</sub> or C<sub>70</sub> efficiently. The present study highlights the differences in recognition behavior that can result from conformational interconversion, as well as providing insights into the basic parameters that govern coupled molecular rotations.