Ni-Fe-Cr-Al alloy has been subjected to a short aging treatment, which increased the mechanical properties and resulted in discontinuous precipitation at the grain boundaries. In this study, analytical electron microscopy was applied to explore the relationship between the occurring grain boundary phenomena and mechanical behavior. Within the discontinuous precipitation zone, three different phases were recognized, namely γ solid solution with lamellar Cr23 C6 carbides and elongated γ’ precipitates at the reaction front. Coherency of the discontinuous precipitates was identified as they have shown a cube-on-cube orientation relationship. Furthermore, the development of multiple discontinuous reactions was discussed.