Peroxymonosulfuric acid preparation

An equimolar amount of peroxymonosulfuric acid, prepared from 90%-H2O2 and coned. H2SO4 added below 15° to a stirred mixture of methacrolein and methanol, stirring continued at 15° for a total reaction time of 3 hrs. methyl methacrylate. Y 97% conversion 90%. F. e. s. A. Nishihara and I. Kubota, J. Org. Chem. 33, 2525 (1968). 

Prepare a solution of peroxymonosulfuric acid, H2SO5, by mixing a little ice-cold concentrated sulfuric acid with potassium peroxydisulfate, keeping the mixture ice-cold for a minute, and then diluting with water. Repeat, with this solution, the tests given above. 

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