Nitric Acid → 1-Nitroanthraquinone

Participants

Reaction Steps

208 g of anthraquinone are introduced into 955 g of 99% nitric acid (mole ratio 15:1) with stirring at room temperature without cooling. When a temperature of 55° is reached, the reaction is continued isothermally until the total reaction time is about 9 minutes. The reaction is then stopped by rapid removal of 376 g of 99% nitric acid by distillation (95.5% nitric acid, γHNO3 = 0.779). Crystallisation is then started by slowly adding 1147 g of 70% nitric acid (crystallisation acid 78.1%, γHNO3 = 0.492). The precipitated product is filtered off, briefly washed with dilute nitric acid, freed from nitric acid adhering to it by evaporation under vacuum and then fractionally distilled at 7 Torr with a head temperature of 275° C. 169.5 g of 98.5% pure 1-nitroanthraquinone (66% of the theoretical amount) are obtained.

Provenance & Evidence