反应详情

温度

55 °C

Pentachlorothiophenol (10.0 g, 0.035 mol) was added to 60.0 g of 99% nitric acid over 20 min at 45°-50° C. followed by heating at reflux (55° C.) for 1.5 hr. At this point 20 mL of 30% by weight oleum was added at such a rate that the temperature was kept at 75° to 80° C. After the addition was complete (approximately 30 min.), the reaction mixture was cooled to room temperature. The product was collected by filtration, and thoroughly washed with water to give after drying in vacuo, 8.6 g (85% yield) of 99.7% PCNB with 0.17% hexachlorobenzene (GC assay). Variations on this one-pot, two-step process were examined and are summarized in TABLE I.

1. temperatureby heating
2. customwas kept at 75° to 80° C
3. additionAfter the addition
4. custom(approximately 30 min.)
5. temperaturethe reaction mixture was cooled to room temperature
6. filtrationThe product was collected by filtration
7. washthoroughly washed with water
8. customto give