Hydrochloric Acid → Quintozene

Participants

Reaction Conditions

Reaction Steps

Into a three-neck 300 ml flask equipped with a mechanical agitator, thermometer and condenser was charged 50 g of 99.7% pure powdered pentachlorobenzene which was heated to 105°-110° C. by means of an oil bath. The flask was then charged with 113 g of mixed nitric acid which contained 16.5% by weight nitric acid and 83.5% by weight sulfuric acid. This mixed nitric acid was gradually added over a period of three hours while the reaction mixture was stirred. Following this addition, the reaction mixture was heated to 125° C. for one hour, followed by further heating at 140° C. for one hour. Then, 7 g of HCl was gradually added over a time period of 15 minutes. After said HCl addition, the reaction mixture was heated again to raise the reaction temperature to 145° C. and to form a liquid melt of pentachloronitrobenzene. The reaction mixture was maintained at this temperature for 15 minutes. Next, the reaction mixture was cooled to 30°-70° C. by removal of the oil bath and by blowing cool air on the flask for about 15 minutes. The reaction mixture was then filtered by suction. The pentachloronitrobenzene product in the filter cake was pressed dry and washed twice with 100 ml water each time. After drying at reduced pressure (20 tor), the product was analyzed by Vapor Phase Chromatography (VPC). In this specific example, the product was of exceptional quality with an assay of 99.20% pentachloronitrobenzene, 0.05% pentachlorobenzene and 0.37% hexachlorobenzene.

Provenance & Evidence