Abstract: For the first time a one step direct conversion of aromatic hydrazines and azo compounds to N-(tert-butoxycarbonyl) amines is achieved via reductive cleavage of NN and N= N bonds using the inexpensive and safe hydride source polymethylhydrosiloxane (PMHS) and di-tert-butyl dicarbonate [(Boc) 2O] in the presence of a catalytic amount of 10% Pd-C. Key words: polymethylhydrosiloxane, hydrazines, azo compounds, tert-butyl ...