Oxacalixcrowns 1, 2 and 3 were synthesized via reactions of dihydroxyoxacalix[2]arene[2]pyrazine S with ortho-, meta- and para-bis（bromomethyl）benzenes in a 1：1 fashion. The structures and conformations of 1, 2 and 3 were established by a combination of NMR, mass spectroscopies and single crystal X-ray diffraction analysis.
