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A modified [3+1] cyclization procedure for the synthesis of calix [4]arenes was developed by using diglycol dimethyl ether as the solvent in place of dioxane which was generally adopted in previous literature. By the modified procedure, the yield of 5-bromo-11, 23-di-tert-butyl-17-methyl-25, 26, 27, 28-tetrahydroxycalix[4]arene from cyclic condensation of 2, 6-bis(2’-hydroxy-5’-tert-butyl-benzyl)-4-cresol and 2, 6-bis (bromomethyl)-4-bromophenol in the presence of TiCl4 was improved from less than 20％ to 40％, and the reaction time was reduced from several days to ten hours.