The degradation of emerging pollutants and dyes using the Fenton reaction can be enhanced by the addition of reducing mediators. This approach helps to minimize the accumulation of Fe(III) in a solution, leading to accelerated Fe(II) regeneration and the increased production of reactive oxygen species, such as the OH radical. In this chapter, we review the effects of hydroxylamine (HA) as a reductant on the Fenton-based oxidation process. The first part critically evaluates relevant literature, emphasizing the advantages and disadvantages of the Fenton-hydroxylamine system and illustrating the redox mechanism. The second part presents a case study on Fenton-hydroxylamine applied to the destruction of two persistent synthetic dyes, where the process's ability to rapidly remove these substances at neutral pH is confirmed. Additionally, we perform a detailed kinetic analysis of the process to optimize its performance under neutral conditions.