P-Phenylenediamine → 1,2,4-Triaminobenzene

Participants

Reaction Steps

A 500 ml autoclave equipped with a stirrer and a gas-introducing tube was charged with 9.5 g of 2,4,4'-trinitroazobenzene, 0.6 g of PtO and 100 ml of ethanol. The inside of the reactor was purged completely with hydrogen, and the reaction was performed at 80° C. for 6 hours with stirring while maintaining the pressure of hydrogen at 70 kg/cm2.G. The reaction mixture was filtered. The cake was washed with water. The wash liquid and the filtrate were combined, and distilled to afford 2.5 g of a fraction having a boiling point of 174° to 180° C./30 mmHg.ab. This fraction coincided with p-phenylenediamine as a standard product. The distillation residue was recrystallized from chloroform to afford 3.2 g of 1,2,4-triaminobenzene having a melting point of 93° to 96° C. This product corresponded in IR spectrum with a standard product.

Provenance & Evidence