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Nano CaCO3 was used as a condensation agent in the ring-opening reaction of p-tert-butylcalix[4]arenc with epichlorohydrin to afford 5,11,17,23-tetra-tert-butyl-26,27,28-trihyd-roxy-25-(1'-chloro-2'-hydroxy-3'-propyl)calix[4]arcne regioseleetively in 52% yield. The yieldwas less than 2% by using normal CaCO3 instead ofnano one under the same conditions.