反应详情

Pentachlorothiophenol (10.0 g, 0.035 mol) was added to 60.0 g of 70% nitric acid at room temperature. The reaction mixture was heated at reflux 7 hr followed by stirring at room temperature 16 hr. At this point, 40 mL of 30% oleum (30% by weight sulfur trioxide in sulfuric acid) was added at such a rate that the temperature was maintained between 55° and 60° C. After the addition was complete (30 min), the reaction mixture was heated at 108° C. for 30 minutes. The reaction mixture was then cooled to room temperature, filtered, the product washed with water and dried in vacuo to give 7.6 g (74% yield) of 99.0% PCNB with 1.0% hexachlorobenzene (GC assay).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux 7 hr
3. temperaturewas maintained between 55° and 60° C
4. additionAfter the addition
5. custom(30 min)
6. temperaturethe reaction mixture was heated at 108° C. for 30 minutes
7. temperatureThe reaction mixture was then cooled to room temperature
8. filtrationfiltered
9. washthe product washed with water
10. customdried in vacuo