Construction of Crystalline Nitrone-Linked Covalent Organic Frameworks Via Kröhnke Oxidation

Developing diverse synthetic routes to prepare various crystalline covalent organic frameworks (COFs) and enrich the family of COFs is very important and highly desirable. In this research, we demonstrate that Kröhnke oxidation (originally developed to prepare carbonyl compounds) can be employed as an efficient method to construct two crystalline nitrone-linked COFs (CityU-1 and CityU-2) through the ingenious design of the polynitroso-containing precursors as well as the exquisite control of the polymerization conditions. The formation and structure of nitrone-based linkage units have been confirmed through a mode reaction. The as-obtained crystalline COFs have been characterized by Fourier transform infrared and X-ray photoelectron spectroscopy, powder X-ray diffraction patterns, and scanning electron microscopy. Notably, CityU-1 exhibits a BET specific surface area of 497.9 m²g^-1 with an I₂ capture capacity of 3.0 g g^-1 at 75 °C. Our research would provide more chances to prepare various crystalline COFs for diverse applications. © 2023 American Chemical Society.