In order to introduce the concept of covalent organic frameworks (COFs), an important class of predictable crystalline porous polymers, an integrated laboratory experiment for advanced organic chemistry students is reported. The importance of these kind of polymers and their multiple applications are presented as a part of key concepts in polymer and organic chemistry, bridging these disciplines to materials science. Students carry out the synthesis and characterization of an imine-linked COF and its building blocks. The polymer is formed at room temperature by using solvent-assisted synthesis and mechanochemistry. Students are trained in solid state characterization techniques, including FTIR spectroscopy, thermogravimetric analysis (TGA),[superscript 13]C NMR cross-polarization--magic angle spinning (CP-MAS) NMR spectroscopy, and powder X-ray diffraction (PXRD), which are essential in the important field of reticular chemistry. Therefore, this lab experience constitutes a practical introduction to COFs.