Synthesis of 2,4-Dinitrotoluene without Nitric Acid

A┬ánitrating solution prepared from 169 g of conc. sulfuric acid and 96 g of oven-dried ammonium nitrate are poured into an addition funnel which is equipped with a reflux apparatus, 50 mL of toluene is poured into the RBF, the condenser doesn’t need to be cooled with water. Slow addition of the nitrating mixture over the course of 3h is started with vigorous stirring, after the addition, the mixture is heated and stirred at 80┬░C for 2h, thereafter cool the solution down and pour the contents into a beaker. The aqueous layer is removed and the crude 2,4-DNT is heated and stirred above its melting point with 250 mL of water, the mixture is cooled down and the water is discarded. The crude product is dried and recrystallized from methanol.

Source

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The apparatus

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Nitration of the toluene

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The mixture poured into water and left to solidify

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The acid waste is discarded and the crude DNT is washed with some water

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Purification of the DNT by melting it with water

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The crude crystals after the melting

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The recrystallized product

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