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The efficiency of a wet chemical route to synthesize gold nanostructures with tunable size and shape significantly depends on the applied solvent and the interaction of solvent molecules with other species such as gold ions. The ability of the organic solvent N-methyl-2-pyrrolidone (NMP) as a suitable medium for application in star-like gold nanostructure (AuNS) synthesis with a tunable morphology at ambient conditions has been investigated. The time-dependent analysis of the UV–vis absorption spectra of AuIIICl₄– in a pure NMP solution illustrates the role of NMP as simultaneous complexing and reducing agents. Kinetic studies indicate that AuIIICl₄– in NMP solution is reduced to AuICl₂–, with no need to use another reducing agent, any external energy sources, or solvent pretreatment. This is because AuI species stay stable in this solution unless poly(vinylpyrrolidone) (PVP) catalyzes their disproportionation. Morphological studies by transmission electron microscopy (TEM) specify the high-yield synthesis of AuNS with monocrystalline spikes in a concentrated NMP solution by PVP. This study illustrates that the presence of seeds, as another agent to catalyze the disproportionation of AuI species, makes it possible to synthesize AuNS in varying concentrations of PVP in this medium. The role of PVP concentration and the presence of seeds in the formation kinetics, morphology, and optical properties is systematically discussed. The results achieved through this study develop a straightforward and safe procedure for AuNS synthesis in high yield in a water-miscible organic polar solvent with tunable morphology and optical properties. Considering the high capability of NMP to dissolve various types of polymers and hydrophobic ligands, synthesizing AuNS in this solvent opens a window to a practical and easy way to fabricate gold-based nanomaterials with fascinating optical properties.