Reaktion #54208
ord-0c2647431ea64ff5af60e3692ef214ed
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1SonstigeInto a three-neck 750 ml flask equipped with a mechanical agitator
- 2Temperaturwas heated to 104°-108° C. by means of an electric heating mantle
- 3Temperaturthe temperature of the mixture maintained at 104°-108° C
- 4workup.ADDITIONthis addition
- 5Temperaturby further heating at 135° C
- 6TemperaturThe reaction mixture was heated again
- 7Temperaturto raise the reaction temperature to above 145° C.
Vorschrift
Into a three-neck 750 ml flask equipped with a mechanical agitator, thermometer and condenser were charged 250 g of 99.7% pure granular pentachlorobenzene and 440 g of 92% sulfuric acid which was heated to 104°-108° C. by means of an electric heating mantle. The flask was then charged with 100 g of 99% pure concentrated nitric acid. This concentrated nitric acid was gradually added over a period of 0.83 hours while the reaction mixture was stirred and the temperature of the mixture maintained at 104°-108° C. Following this addition, the reaction mixture was heated to 125° C. for one hour followed by further heating at 135° C. The reaction mixture was heated again to raise the reaction temperature to above 145° C. and to form a liquid melt of pentachloronitrobenzene. The reaction mixture was maintained at this temperature for about 30 minutes. Next, the reaction mixture was cooled to 30°-70° C. by switching off the heating mantle and blowing cool air on the flask for about 30 minutes. The reaction mixture was then filtered by suction. The pentachloronitrobenzene product in the filter cake was washed twice with about 500 ml of distilled water each time. After drying at room temperature for 24 hours, the product was analyzed by Vapor Phase Chromatography (VPC). In this specific example, the product was of exceptional quality with an assay of 99.74% pentachloronitrobenzene, less than 0.01% pentachlorobenzene and 0.26% hexachlorobenzene.