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In this work, we report the preparation of Al2O3/V2O5 nanocomposit using vanadium and aluminum nitrate by sol-gel method. Characterization of nanocomposit was carried out by powder X-ray diffractometry (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), Energy-Dispersive X-ray (EDX) and UV spectroscopy. Then, applicability of the synthesized nanocomposit was tested as a nanocatalyst for the synthesis of diindolyl oxindole derivatives, an important class of potentially bioactive compounds. The products were obtained in good to high yields from one-pot three-component condensation of isatin with indole. Also, this nanocatalyst has been reused several times, without observable loss of activity. [ABSTRACT FROM AUTHOR]