Rapid Synthesis of High Surface Area Imine‐Linked 2D Covalent Organic Frameworks by Avoiding Pore Collapse During Isolation

sorption and X-ray diffraction. This loss of material quality during isolation for many networks has historically obscured otherwise effective polymerization conditions. The influence of the activation procedure is characterized in detail for three COFs, with the commonly used 1,3,5-tris(4-aminophenyl)benzene-terephthaldehyde network (TAPB-PDA COF), the most prone to pore collapse. When the networks are activated carefully, rapid COF formation is general for all five of the imine-linked 2D COFs studied, with all exhibiting excellent crystallinity and surface areas, including the highest surface areas reported to date for three materials. Furthermore, to simplify the workup of COF materials, a simple nitrogen flow method provides high-quality materials without the need for specialized equipment. These insights have important implications for studying and understanding how 2D COFs form.