Biologically portent/significant tetrahydrodipyrazolo[3,4‐b:4′,3′‐e]pyridines are synthesized by an efficient green synthesis of various aldehydes with 3‐methyl‐1H‐pyrazol‐5(4H)‐one in ammonium acetate using phospho sulfonic acid as a solid catalyst under microwave‐assisted interaction under solvent‐free conditions at 70°C. This methodology is easy to handle and get good to excellent yields. Later the potential in vitro antiproliferation of the titled compounds is evaluated. Among all the titled compounds, 4s and 4t showed the most potent anticancer potentiality on the used cancer cell lines of SK‐BR‐3 and HeLa (IC50 = 10.70 ± 0.27 and 12.58 ± 0.38, and 19.38 ± 0.32 and 21.55 ± 0.41 μg/mL for SK‐BR‐3 cells lines and HeLa cells lines, respectively), which were comparable to the positive control.
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