An undergraduate laboratory experiment for the synthesis of biologically significant bis-4-hydroxycoumarins using a new catalyst is described here. An experimental setup plan, monitoring the reaction by TLC, isolation of the product, safe laboratory handling procedures, and significance of data reproducibility of the result are the main learning outcomes of this work. The products are characterized by melting point, [superscript 1]H nuclear magnetic resonance (NMR), [superscript 13]C NMR, distortion enhancement by polarization transfer (DEPT) NMR, and Fourier transform infrared (FTIR) spectra. This simple and cost-effective experiment with wide substrate applicability also introduces the concept of research work on multicomponent condensation reaction among the students.