Convenient Synthesis of Geminal Bishydroperoxides by the Reaction of Ketones with Hydrogen Peroxide

A convenient procedure was developed for the synthesis of geminal bishydroperoxides by the sulfuric acid–catalyzed reaction of ketones with hydrogen peroxide in THF. Gem‐bishydroperoxides were prepared by the reactions of five‐ to seven‐membered cycloalkanones without additional purification in 80–95% yields with a purity of more than 95%; their acyclic analogs were prepared in 43–72% yields.