1-Alkyl-3-p-tolytriazenes were used to synthesize the methyl, ethyl, isopropyl and benzyl esters of bilirubin. Treatment of a chloroform solution of bilirubin with the triazene at room temperature gave high yields of the corresponding esters. These were identified by n.m.r. and mass spectroscopy together with elemental analysis. N.m.r. studies also suggest that bilirubin dimethyl ester is in the lactam rather than the lactim form.