Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzonitrile | HCID 7505 | — |
| Reactant | HCID 22467808 | HCID 22467808 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Catalyst | Cuprous chloride | HCID 62652 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22467812 | HCID 22467812 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06384167B2 |
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| Source dataset | uspto-grants-2002_05 |
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| ORD ID | ord-39705c6d6c3b40a087a64d098660dea1 |
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| Source note | uspto-grants-2002_05 |
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