The reactions of ketones 1a–o, nitromethane 2, and a stoichiometric amount of piperidine 3a or ethylenediamine 3b in the presence of mercaptan 6a in THF or CH3CN solution give high yields of β-nitrosulfides 7a–o. The latter can be oxidized by 8a (m-CPBA or m-CPBA/AcOH) at 0° C, 8b (H2O2/AcOH), or 8c (H2O2) at room temperature, thus generating β- nitroalkylsulfoxides 9a–o, which then undergo elimination to produce medium to high ...