Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Hexanol | HCID 8103 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-[Bis(trifluoromethanesulfonyl)methyl]-2,3,4,5,6-pentafluorobenzene | HCID 10203986 | — |
| Reactant | Hydrate;hydrochloride | HCID 21885828 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 23249444 | HCID 23249444 | 99% |
Reaction Steps
Hexanol (1.5 mL, 12 mmol) was added to a pyridine (10 mL) solution dissolved with 60% sodium hydride containing mineral oil (0.56 g, 14 mmol) at 0° C., and the resultant solution was stirred for 1 hour at room temperature. After the solution was cooled to −20° C., pentafluorophenylbis(triflyl)methane (0.89 g, 2 mmol) was added. The reaction solution was stirred at −20° C. for 5 hours. After the reaction, the solution was acidified with 4 M hydrochloric acid water, and was extracted with diethylether. After drying with magnesium sulfate, the solution was filtrated, and the solvent was removed under reduced pressure. The crude product was purified by sublimation (0.2 to 0.3 torr, 65° C.), and 4-hexanoxy-2,3,5,6-tetrafluorophenylbis(triflyl)methane was obtained at 99% yield (1.02 g, 1.98 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07193113B2 |
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| Source dataset | uspto-grants-2007_03 |
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| ORD ID | ord-7775c2c50eb640adbe1d3b7b967176fc |
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| Source note | uspto-grants-2007_03 |
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