Two different azosulphonate dyes were synthesised and purified for the preparation of a water-based photoreactive azosulphonate-doped poly(vinyl alcohol). The aim was the investigation of a novel azosulphonate-poly(vinyl alcohol) photoresist with decreased water solubility after illumination, setting a focus on environmentally benign substances. The electron distribution of the aromatic rings of the two different azosulphonate molecules were changed by the UV-induced cleavage of the ⁻N=N⁻SO₃- groups, which was evidenced by UV spectroscopy. The formation of ester groups was detected by Fourier-transform infrared and 13C nuclear magnetic resonance spectroscopy. UV⁻Vis spectroscopy was used to investigate the photoreactivity of the prepared films. Photolithographic experiments demonstrated the applicability of these newly produced materials as photoresist materials. In addition, these materials provide high thermal stability.