Di- and tetrasubstituted p-tert-butylthiacalix[4]arene in three different conformers (cone, partial cone and 1,3-alternate) at lower rim, have been synthesized by the reaction of p-tert-butylthiacalix[4]arene and disubstituted p-tert-butylthiacalix[4]arene with isatin-3-[N2-(chloroacetyl)]hydrazone in acetone or acetonitrile in the presence of different alkali metal carbonates or hydroxide. Structures of the new compounds were established by elemental analyses and spectral data IR, 1H NMR, 13C NMR