Sulfuric Acid → 4-Nitro-m-phenylenediamine sulfate

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Reaction Steps

In an agitated glass-reaction vessel, 50 g. of 4-nitro-m-phenylenediamine is added to 200 g. of isopropanol. While maintaining the temperature below 50 deg. C., 110.0 g. of conc. sulfuric acid is added to the mixture to a pH of 2.0.±0.5. After the acid addition, the mixture is heated to between 70-75 deg. C for 3 hours. After 3 hours, the batch is cooled down to below 30 deg. C. and then agitated for another hour. The product is filtered, washed with water, and dried under conditions below 80 deg. 77-80 g. of 4-nitro-m-phenylenediamine sulfate is obtained resulting in a yellow-brown powder. A 94-97% theoretical yield is obtained relative to 4-nitro-m-phenylenediamine.

Provenance & Evidence