Abstract An efficient one-pot procedure for the zinc-mediated reduction of nitroarenes in the presence of chloroformates leading to the corresponding N, O-bisprotected hydroxylamine is described. Reactions proceed smoothly under ambient conditions in THF-water mixtures in good to excellent yield (34-81%). Solvolysis of the bisprotected hydroxylamines with sodium methoxide at room temperature provides access to synthetically versatile N-aryl-N- ...