Abstract: Some 4, 4'-disubstituted-diazoamino-benzenes with possible schistosomicidal activity have been prepared by coupling p-substituted benzene diazonium salts with substituted anilines in weak acidic solution. The preparation of p-nitro-β-hydroxy ethyl aniline was improved by using freshly prepared copper powder as catalyst. Two intermediates, p-N-β-acetoxy ethyl-N-acetamino aniline and p-N-β-diethylamino ethyl-N-acetamino aniline, were also reported.