A new and simple synthesis is described for N-acetoxy-N-acetyl-derivatives of trans-4-aminostilbene, 2-aminofluorene and 2-aminophenanthrene using a Zn/Cu-couple for the reduction of the nitro-aromatics. This method produces good yields and should also be applicable for other N-aryl-compounds. It can also be used for the reduction of nitro-aromatics to the respective arylamines and arylamides.