The formation of mono- and di (1,2 and 1,3)-amide derivatives of p-tert-butylcalix[4]arene in the presence of sodium hydride has been demonstrated. All the compounds have been purified and characterized by various spectral methods. Both 1H and 13C NMR spectra exhibit clear-cut differences between the 1,2-di- and 1,3-di-amide derivatives.