Nitric Acid → 1-Nitroanthraquinone

Participants

Reaction Steps

208 g of anthraquinone are introduced into 764 g of 99% nitric acid (mole ratio 12:1) at room temperature with stirring. The reaction is then left to proceed adiabatically until the temperature reaches 45°. The reaction is then continued isothermally at 45° until the total reaction time is 17 minutes. The reaction is stopped by distilling off 330 g of 99% nitric acid. 128.0 g of 50% nitric acid (crystallisation acid 83.4%, γHNO3 = 0.542) are slowly added to the sump product (acid concentration approximately 94.4%, γHNO3 = 0.725). The product which precipitates under these conditions is suction-filtered, washed with a little dilute nitric acid, freed from nitric acid by washing with water, dried and subjected to vacuum rectification at 8 Torr with a head temperature of 275°. 162.3 g of 98.2% pure 1-nitroanthraquinone are obtained as a distillate (63% of the theoretical amount).

Provenance & Evidence