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Iodination of various industrially and pharmaceutically important substituted aromatics has been achieved using N-iodosuccinimide (NIS) in solid state by grinding at room temperature. This method provides several advantages such as short reaction time (5–8 min), high yields (94–99%), and nonhazardous and simple work-up procedure. High gas chromatography (GC) purity (95–99.9%) suggests that the reaction is highly selective. Substrates which are sensitive to oxidation, viz aniline and phenols are iodinated smoothly in high yield.