Single-Pot Synthesis and Optimization of CCF@GO Nanocatalyst for Efficient Direct Oxidative Amidation of Carboxylic Acids and N,N-Dialkylformamides

Abstract

In this study, an efficient catalytic protocol using CuCoFe₂O₄@GO (CCF@GO) for the synthesis of amide bond (−CONH−) via direct coupling of carboxylic acids and N,N-dialkylformamides is presented. The CCF@GO nanocatalyst has been synthesized via a single-pot solvothermal method, by changing the proportions of copper and cobalt (1:1, 1:3, and 3:1). Catalyst screening, employing a model reaction with benzoic acid and dimethylformamide (DMF), revealed that the 1:1 proportion of CCF@GO catalyst exhibited excellent efficiency, achieving a high conversion (98%) towards amide formation. The enhanced catalytic efficiency observed in CCF@GO catalysts can be ascribed to the uniform distribution of active copper and cobalt species on the graphene oxide support, which possesses a high surface area. Optimization of the reaction was conducted by varying parameters such as temperature, solvent, catalyst loading, and oxidant. The prepared catalyst was characterized using various analytical techniques including XRD, FTIR, XPS, SEM, EDX mapping, and TEM. Furthermore, this heterogeneous nanocatalyst demonstrated recoverability using an external magnet and reused up to five times with just a modest loss of catalytic performance.