Selective Anodic Oxidation of Solketal as Acetal‐Protected Glycerol over Nickel Boride in Alkaline Media to Glyceric Acid**

Alkaline anodic oxidation of glycerol suffers from facile C−C bond cleavage, especially when using non-precious metal electrocatalysts, which limits the yield more valuable C3 oxygenates. Usually, a high selectivity is tradeoff with conversion for most catalysts. Thus, we used solketal as reactant, acetal-protected acetone. CV experiments showed that oxidized over nickel boride (NixB) at potentials where NiOOH formed. Electrolysis NixB in thin-film spectroelectrochemical flow cell 1.58 V vs. RHE to avoid pronounced oxygen evolution stable current density ca. 6 mA cm−2. Simultaneously recorded ATR-FTIR spectra revealed solketalate and formate. Indeed, 59 % 77 glyceric acid were determined by HPLC after acidic cleavage acetal, resulting 45 %. Therefore, promising reactant selective electrosynthesis acid.