Process for preparing radicals N-oxides of secondary amines (radical nitroxides) from the corresponding secondary amines, characterized in that the following steps are performed: a / the secondary amine is dissolved with an organic solvent immiscible with water, and then water is added, b / is then added, simultaneously and under so vigorous stirring, the biphasic medium thus obtained, an amount of an aliphatic peracid according to a molar ratio of peracid to secondary amine is 1, 5 to 2, 5, and a sufficient amount of an aqueous basic solution to obtain a pH of the aqueous phase of the biphasic medium is 4 to 12, at a temperature between -10 yy + 40 ° C, until conversion of the amine lacompleta secondary, and then c / the organic phase by simple decantation is recovered, and the nitroxide is isolated by evaporating the organic solvent under reduced pressure.
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