Nontoxic and energy‐efficient COF synthesis: Covalent organic framework TpPa‐1 has been successfully obtained in a microwave‐assisted hydrothermal synthesis, replacing the traditional organic‐based solvent with water and reducing reaction times from several days to 30 minutes. High‐temperature hydrothermal synthesis resulted in higher BET specific surface areas (compared to traditional solvothermal processes), improved material yields, and excellent textural properties. More information can be found in the Research Article by B. Zornoza, C. Téllez, and co‐workers (DOI: 10.1002/chem.202203907).

Three synthesis procedures for the covalent‐organic framework (COF) TpPa‐1 are studied with the purpose of setting up the most promising one in a fast and green way, leading to a more environmentally friendly and sustainable process. With conventional heating, good crystallinity and a high BET specific surface area (SSA) of up to 1007 m2 ⋅ g−1 are achieved at 170 °C for 3 days using water as the quintessential green solvent. However, the application of microwave radiation in the synthesis for this crystalline porous polymer allows reaction times to be shortened to 30 min while maintaining structural and textural properties (BET SSA of 928 m2 ⋅ g−1) and obtaining yields close to 98 % (vs. 90 % in the hydrothermal synthesis). The water‐assisted mechanochemical synthesis is also an environmentally friendly synthetic approach; with heating at 170 °C in a two‐step process (10+10 min), high crystallinity is achieved, a BET SSA of 960  m2 ⋅ g−1 and a yield of 98 % for TpPa‐1.