Abstract: Diastereomeric a-disulfoxides (14) have been detected as intermediates in the m- chloroproxybenzoic acid (MCPBA) oxidation of neopentyl neopentanethiosulfinate (6) at-40 OC in CDC13 via'H NMR and I3C NMR spectroscopy. The product mixture at-40 OC contained 6, 14, neopentyl neopentanethiosulfonate (7), and neopentanesulfinic acid (11). Oxidation of 6 at-20 OC, followed by warming to 0 OC and treatment with NaHC03, gave ( ...