ABSTRACT

The reduction of nitroaromatic compounds is well known and the reaction kinetics have been extensively studied. The main reaction proceeds in three consecutive steps: first hydrogenolysis, hydrogenation, and second hydrogenolysis. The choice of a tertiary compound was selected to avoid the potential equilibrium between the nitroso and the oxime (which could occur with secondary and primary nitroso compounds). Calibration mixtures of MNP, MNoP, TBHA, TBA with the chromatographic standard were prepared. These synthetic mixtures were put into the autoclave, standard stirring was applied, and the standard sampling procedure was followed. For the catalytic reaction, concentrations of reactant, intermediates, and product were plotted versus time. The reactant curve was fitted to yield the reaction rate, e.g., when TBHA was the initial reactant. Tertiary aliphatic nitroso compounds were found to be very quickly reduced in a hydrogen atmosphere, even in homogeneous solution without a catalyst.