In this study, several novel sterically congested silicon and titanium bisenolates of exceptional hydrolytic stability have been synthesized and characterized. The structure of the titanium bisenolate T2 could be determined by X-ray structure analysis. Preparative one-electron oxidation of the stericallyshielded metal bisenolates S1-S4 and T1-T2 led to formation of the benzofurans B1 and B2. As the