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Abstract A practical preparation of nitroarylamines from protected arylamines was herein disclosed. In this system, sodium nitrite acted as a nitration reagent in the presence of sodium persulfate without any transition-metal catalysts. This efficient site-selective protocol took place at room temperature for a short time through a free radical pathway. Graphical abstract A site-selective preparation of nitroarylamines was herein disclosed from protected arylamines and sodium nitrite in the presence of Na 2 S 2 O 8 without any transition-metal-catalysts. The mild protocol took place at room temperature for a short time through a free radical mechanism with broad substrate scope and high efficiency. Image 1 [ABSTRACT FROM AUTHOR]