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A novel series of N-alkylphthalimidylaminocarbonylmethoxylcalix[4]arenes with the reaction between 4-(N-bromoacetylamino)-phthalimide derivatives and calix[4]arene has been synthesized and structurally characterized by IR, 1H NMR and MS. From their analysis data, it was found that compounds 7a-7d adopted a cone conformation.