Formylation of 2, 7-di-tert-butylpyrene with dichloromethyl methyl ether in the presense of AlCl3 afforded a mixture of 2, 7-di-tert-butylpyrene-4, 9-biscarbaldehyde and 4, 10- biscarbaldehyde in the ratio of 75: 25, from which the corresponding bis (arylethynyl) pyrenes were obtained by the Wittig reaction with aryl methyl phosphonium ylides followed by bromination and dehydrobromination.