Hybrid composite based on graphene oxide (GO) and covalent organic framework (COF) [GO/COF] was developed via a simple solvothermal method, at which GO was applied as a platform to load COF based on melamine and terephthaldehyde. The synthesized hybrid nanocomposite was characterized by FT‐IR, XRD, EDX and SEM techniques. Morphological analyses carried out by SEM confirm the successful growth of COF over GO. Then, the resultant composite was employed as an amazing and cost‐effective catalyst in the condensation of several aldehydes with malononitrile and produced the corresponding coupling products in high yields (up to 84%) at room temperature under solvent‐free conditions with an amount of catalyst, 15 mg in a very short reaction time of 10 min. The catalyst could be reused without a noteworthy drop in catalytic activity at least eight times. The use of GO/COF catalyst outcomes under mild reaction conditions in very short reaction time, exceptional catalytic activity, high recyclability and an easy work‐up process for the Knoevenagel condensation.
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