In acetonitrile containing tetraethylammonium perchlorate, cyclic voltammograms for the reduction of 2,4,6-trimethylbenzoyl chloride at glassy carbon and hanging mercury drop electrodes exhibit five and four cathodic waves, respectively. At potentials corresponding to the first wave, cleavage of the carbon-chlorine bond occurs to generate acyl radicals and anions that lead to the formation of 2,4,6-trimethylbenzaldehyde, and the second wave is due to reduction of the aldehyde. Controlled-potential electrolyses of 2,4,6-trimethylbenzoyl chloride at a potential on the foot of the first wave produce 2,4,6-trimethylbenzaldehyde and a tetrameric species, along with hydrolytically formed 2,4,6-trimethylbenzoic acid and 2,4,6-trimethylbenzoic anhydride. However, at a potential more negative than the peak potential for the first wave, co-reduction of some of the aldehyde takes place, yielding 2,4,6-trimethylbenzyl alcohol and 1,2-bis(2,4,6-trimethylphenyl)-1,2-ethanediol, plus products that incorporate the solvent : 3-hydroxy-3-(2,4,6-trimethylphenyl)propionitrile, 3-(2,4,6-trimethylphenyl)acrylonitrile, 3-(2,4,6-trimethylphenyl)propionitrile, 3-(2,4,6-trimethylphenyl)glutaronitrile, 2,3-bis(2,4,6-trimethylphenyl)-1,4-dicyanobutane, and 1-amino-2-cyano-3,4-bis(2,4,6-trimethylphenyl)cyclopent-1-ene. Separate cyclic voltammetric studies and controlled-potential electrolyses of 2,4,6-trimethylbenzaldehyde have confirmed these findings.