Experimental protocol for the study of One-pot amination of Cyclohexanone-to-secondary amines over Carbon-supported Pd

The validation of protocols for carrying out the experimental analysis of amination reactions is of paramount importance to enhance the scientific knowledge and reproducibility of results. Accordingly, in the present paper, a protocol has been proposed for the study of the amination of cyclohexanone-to-secondary amines (Diphenylamine and N-Cyclohexylaniline) over heterogeneous catalysts. The results of activity and selectivity, and the elucidation of a plausible reaction pathway were described in a parent paper. Therefore, the purpose of this document is to inform about the details of the experimental setups, the methods, and the analytical techniques to identify and quantify the reaction products. Finally, some practical and safety considerations are also included. One-pot catalytic amination of cyclohexanone with aniline was performed efficiently in liquid phase on Pd/C. Stirring, He atmosphere and temperature control were critical to achieve reproducible activity results. Ultra-High Performance Liquid Chromatography allows identifying products and reaction intermediates, while nonane performed well as internal standard for GC-FID quantification. (C) 2021 The Author(s). Published by Elsevier B.V.