The p-tert-butylcalix[4]arene (1) was firstly alkylated with 1,2-dibromoethane and 1,3-dibro- mopropane to give calix[4]arene derivatives 2 and 3 in the presence of potassium carbonate, respectively. A series of p-tert-butylcalix[4]arene derivatives 4a～4c, 5a～5c which append thiadiazolidinyl groups at the lower rims were easily synthesized in good yields by the reaction of compounds 2 or 3 with 2-mercapto- thiadiazole. All new compounds were characterized by ¹H NMR, ¹³C NMR, IR, MS spectra and elemental analysis.

Key words: synthesis, characterization, thiadiazole, calix[4]arene derivative