Sulfuric Acid → 4-Nitro-m-phenylenediamine sulfate

Participants

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. After the acid addition, the mixture is heated between 70-75 deg. C for 3 hours, to a pH of 2.0±0.5. After 3 hours, the batch is cooled down to below 30 deg. C and then agitated for another hour. The product is filtered and dried under conditions below 80 deg. C. 78-81 g. of 4-nitro-m-phenylenediamine sulfate is obtained resulting is a yellow-brown powder. A 95-98% theoretical yield is obtained relative to 4 nitro-m-phenylenediamine.

Provenance & Evidence