Broadly applicable synthesis of 1,2,4,5-tetraoxanes.

Re(2)O(7) is a mild and efficient catalyst for the high-yielding condensation of 1,1-dihydroperoxides with ketones or aldehydes to form 1,2,4,5-tetraoxanes, including targets not easily prepared via existing methodology. When applied in tandem with a recently reported Re(VII)-catalyzed synthesis of 1,1-dihydroperoxides, the reaction provides a high-yielding one-pot conversion of ketones or aldehydes to tetraoxanes.