Abstract Upper-rim modification of tetramethylcalix [4] resorcinolarene with 3, 5-di-tert-butyl- 4-hydroxybenzyl fragments is accompanied by unusual decomposition of the macroring in the modified product with formation of 2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) resorcinol.