The preparative scale synthesis of dimesityldioxirane (5) via oxidation of dimesitylcarbene (6) is described. The dioxirane was obtained as colorless crystalline material, completely stable at -20 deg C and characterized by spectroscopic methods, X-ray crystallography, and DFT calculations (B3LYP/6-31G(d)). The molecule shows approximately local C_2 symmetry with the mesityl rings twisted by ca.60 deg.
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