The azo-ester compounds containing an acryloyloxy group were derived from phenol and 2,6-dimethylphenol; first azobenzene derivatives were prepared by reacting substituted benzenediazonium salts with phenol and 2,6-dimethylphenol then their acryloyloxy derivatives were synthesized in a Schotten-Bauman-type reaction. The characterisation of the synthesized azo-ester dye has been described by IR, UV-vis, H-1 NMR, C-13 NMR spectroscopic techniques, and elemental analysis. The influence of the substituents and acryloyloxy group on the spectral data of the synthesized compounds has been described. The thermal behaviour of the present compounds has been determined by means of differential thermal analysis (DTA) and thermogravimetry (TG) techniques. (c) 2005 Elsevier Ltd. All rights reserved.