Abstract Resorcinarene O-acetates, which are key intermediates in the chemical modification process of resorcinarene, can be efficiently prepared in high yields by BF 3· OEt 2 catalyzed cyclocondensation of 1, 3-(dialkoxycarbonylmethoxy) benzenes with aromatic or aliphatic aldehydes in CH 2 Cl 2 at room temperature. The single crystal structure analysis indicates alkyl resorcinarenes prefer rccc configuration, while aryl resorcinarenes usually ...