Abstract 1, 4-Diketones were prepared by cerium-catalyzed oxidative coupling of styrene with molecular oxygen and 1, 3-dicarbonyl compounds. This two-step sequence was performed as a one-pot procedure without isolation of the intermediate products. The first step is a metal-catalyzed radical reaction yielding 3-hydroxy-1, 2-dioxane derivatives being the cyclotautomers of initially formed 4-hydroperoxy ketones. In the second step of this ...