We report the results obtained by direct metalation of aromatic tertiary diamines with n-BuLi. The reaction done in a nonpolar solvent, such as hexane, at elevated temperature (60°C) shows the formation of both a mono-lithiated and a dilithiated compound, the site of lithiation being the ortho position of the benzene ring as evidenced by 1H NMR data. The metalation was followed by gas chromatography by measuring the butane evolved during the reaction. Copyright © 1979, American Chemical Society. All rights reserved.