Excision in Reduced Dimensionality: Synthesis of 1D Covalent Organic Framework via Clip‐off Chemistry

Synthesizing 1D COFs with a tailored chain stacking model is a significant challenge. Here, we introduce a novel preparation approach of 1D COFs involving selective excision from 2D matrix via clip‐off chemistry. We carefully designed a 2D sql framework incorporating strategically cleavable olefinic linkers, enabling transformation of X‐shaped tetratopic linkers into V‐shaped ditopic counterparts through ozonolysis. The resulting 1D COF, featuring carboxyl group, was then functionalized with Anderson‐type POMs via Schiff base reactions. This POM‐COF composite demonstrated enhanced photocatalytic aldehyde oxidation, benefiting from synergistic effects to achieve efficient and selective conversion of aldehydes to carboxylic acids. Our work offers valuable insights for the custom synthesis of 1D COFs with predefined chain arrangements and functional orientations.