Benzonitrile → HCID 22467812, compound

Temperature

110 °C

Into a 250 ml of round bottom flask were placed 16.5 g (0.03 mol) of the 2,4-di(2-bromotetrafluoroethoxy)benzenesulfonyl fluoride, 5.94 g (0.06 mol) of copper(I) chloride and 6.54 g (0.1 mol) of activated zinc powder. Then 120 mL of well-dried benzonitrile was added to the mixture. The solution was stirred at 110° C. for 2 days with the protection of dry nitrogen gas. After being cooled down to room temperature, 120 mL of methylene chloride was added to the flask and the mixture was stirred at that temperature for eight hours, followed by filtration to remove the solid materials. Then 5 g of active carbon was added to the filtrate and the mixture was refluxed for overnight. After being cooled down to room temperature, the mixture was filtered to remove active carbon and the solvents were removed under the reduced pressure. The crude material was purified by sublimation at 120° C. oil bath temperature at 10−2 torr to give 2,4-di(trifluorovinyloxy) benzenesulfonyl fluoride, identified by 19F and 1H NMR.

1. customInto a 250 ml of round bottom flask were placed
2. temperatureAfter being cooled down to room temperature
3. stirringthe mixture was stirred at that temperature for eight hours
4. filtrationfollowed by filtration
5. customto remove the solid materials
6. additionThen 5 g of active carbon was added to the filtrate
7. temperaturethe mixture was refluxed for overnight
8. temperatureAfter being cooled down to room temperature
9. filtrationthe mixture was filtered
10. customto remove active carbon
11. customthe solvents were removed under the reduced pressure
12. customThe crude material was purified by sublimation at 120° C. oil bath temperature at 10−2 torr

ORD record

ord-39705c6d6c3b40a087a64d098660dea1

Source dataset

uspto-grants-2002_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06384167B2