Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Reactant | 1,7,8-Trifluoronaphthalen-2-ol | HCID 23077306 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23077305 | HCID 23077305 | — |
Reaction Steps
Pyridine (10 ml) was added slowly and dropwise to a dichloromethane (60 ml) solution of 1,7,8-trifluoro-2-naphthol (10 g) and trifluoromethanesulfonic acid anhydrate (10.3 ml) at the temperature of the ice/water, and then the reaction solution was stirred for 30 minutes. Water and dichloromethane were added slowly in the reaction solution. The organic layer was removed, and the aqueous layer was extracted with dichloromethane. The organic layers were combined, washed with water, 10% hydrochloric acid, a saturated sodium hydroxide aqueous solution, water, and brine consecutively, and concentrated. The residue was purified by column chromatography (silica gel, hexane/ethyl acetate=19/1), and 1,7,8-trifluoronaphthalene-2-yl trifluoromethanesulfonate was obtained as light yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07214835B2 |
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| Source dataset | uspto-grants-2007_05 |
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| ORD ID | ord-ee7ad5da31a64fbcafa54725ac7d2db7 |
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| Source note | uspto-grants-2007_05 |
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