The synthesis of oligomeric arylamides was carried out in a reaction calorimeter by low temperature interfacial polycondensation. The on line measurements of the evolved heat under different reaction conditions allowed us to estimate both kinetic and thermodynamic parameters. A complex mechanism seems to take place, involving the formation of co-monomeric species, their coupling and/or the monomeric attach on the initially formed condensation product. A proper choice of both the synthetic procedure and the related experimental parameters (temperature, concentration of reagents and their initial molar ratio, stirring rate, etc.), allows to induce structural modifications in the resulting oligomeric species. The process was optimized in terms of yields, distribution of end groups and average molecular masses, as a function of thermochemical data.
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