During the course of our studies on calixarene chemistry,11we recently introduced bisresorcinarenes 1a−d, which arecomposed of two resorcinarenes connected with four aliphaticchains in a feet-to-feet fashion (Figure 1), as a versatile scaffoldsfor homoditopic hosts.12 The intermolecular rim-to-rimhydrogen bonding of 1a−d produced hydrogen bondedsupramolecular polymers. The upper-rim functionalization of1a and 1c with phosphonate groups produced phosphonatebridged biscavitands, which demonstrate allosteric regulation inammonium guest binding.13 1a−d were synthesized throughmulticomponent condensation reactions with eight resorcinolmolecules and four flexible dialdehydes molecules; however,this reaction suffered from extremely poor chemical yields.Bis(dimethoxy acetals) were developed to be latent alternativesto the dialdehydes, but the product yields remained moderate.Therefore, an improvement in the reaction conditions washighly important.