Abstract: Single 2-butyne-bridged and double 2-butyne-bridged biscalix[4]arenes were prepared directly by the reaction of p-tert-butylcalix[4]arene with 1,4-dichloro-2-butyne using K₂CO₃^- as a base in acetonitrile. It was found that the double 2-butyne-bridged biscalix[4]arene was formed via 2-butyne-single bridged biscalix[4]arene. Their structures were characterized by ¹HNMR, ¹³CNMR and ESI-MS. They exhibited different complexion ability towards DMF and H₂O molecule.

Key words: Calix[4]arene, Biscalix[4]arene, 1,4-Dichloro-2-butyne, Bridging