Pyrogallol cyclic tetramers, tetrasulfonated pyrogallol cyclic tetramers and 25, 27-di(3, 4, 5-trihydroxybenzoyloxy)dihydroxy-calix[4]arene were synthesized. The calix[4]arenes emit light in the presence of hydrogen peroxide in an alkaline medium. Of three calix[4]arenes, 25, 27-di(3, 4, 5-trihydroxybenzoyloxy)dihydroxy-calix[4]arene gave the highest chemiluminescence intensity, and the intensity of the calix[4]arene was 190-fold greater than that of gallic acid in the same solvent.