Optically active nitroxyl radicals are prepared from enantiomerically pure bicyclic terpenoids.(−)-Camphoxyl radical (−)-4 derived from commercially available oxazolidinone ((−)-1) and (+)-camphoxyl radical (+)-4 derived from (−)-camphene are readily prepared, conformationally rigid, enantiomeric nitroxyl radicals.(−)-Camphorsulphonic acid is used to prepare two additional optically active nitroxyl radicals 9 and 12.