Group VA metalloid ion Lewis acids, Sb(V) was identified as a highly potent catalyst for the one-pot three-component synthesis of bis-spiro piperidine derivatives. The reaction was performed using amines, formaldehyde, and dimedone under ultrasonic irradiation at room temperature. The strong acidic property of the nano γ-alumina supported antimony(V) chloride plays a key role in accelerating the rate of the reaction and initiates the reaction smoothly. The heterogeneous nanocatalyst was fully characterized by FT-IR spectroscopy, XRD, EDS, TGA, FESEM, TEM, and BET techniques. Also, the structures of the prepared compounds were characterized by ¹H NMR and FT-IR spectroscopies.