Abstract A chiral spin trap, 5, 5-dimethyl-3-phenylpyrroline-1-oxide (5), and several hydroxylamines were synthesized. The structures and conformations of these compounds were investigated mainly by 1 H NMR spectroscopy. This spin trap was used to trap carbon- and oxygen-centered radicals. The corresponding hydrogen spin adduct was prepared by oxidizing the hydroxylamine to the nitroxide radical. By the combination of 1 H NMR and ...