Hydrogen Peroxide → 2,3,3-Trimethylbutane-2-peroxol

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Reaction Steps

A 300-ml four-necked flask equipped with a stirrer, thermometer and dropping funnel was charged with 73.7 g of a 50% hydrogen peroxide aqueous solution. Stirring was started, the flask was kept at a temperature below 20° C. by water cooling, and 51.7 g of 98% conc. sulfuric acid was added dropwise to form a mixed acid. While the flask was cooled at a temperature of 0° to 5° C. with an ice bath, with stirring, 40 ml of a dichloromethane solution containing 42.9 g of 1,1,2,2-tetramethylpropyl alcohol which was previously synthesized according to Journal of the American Chemical Society/89:7/Mar. 29, 1967, was slowly added dropwise. At the end of addition, stirring was continued for a further 2 hours. The reaction solution was washed with pure water until the organic layer became neutral. The organic layer was dried over anhydrous sodium sulfate and distilled of the solvent, yielding 47.4 g of 1,1,2,2-tetramethylpropylhydroperoxide having structural formula (2).

Provenance & Evidence