HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoromethanesulfonic anhydride → 2-Acetyl-4-fluorophenyl trifluoromethanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | 2-Acetyl-4-fluorophenol | HCID 95992 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 2-Acetyl-4-fluorophenyl trifluoromethanesulfonate | HCID 59717614 | 101.4% |
Reaction Steps
Trifluoromethanesulfonic anhydride (8.6 mL, 51 mmol) was added dropwise at 0° C. to a stirring solution of 5′-fluoro-2′-hydroxy-acetophenone (6.4 g, 41 mmol) in pyridine (62 mL). The reaction was stirred overnight from 0° C. to ambient temperature. The reaction solution was diluted with diethyl ether (500 mL). The organic layer was washed with 1 N aqueous hydrochloric acid (1×300 mL), followed by a saturated, aqueous sodium chloride solution (2×300 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to give a maroon-colored liquid (11.9 g, 100% ). The product was further purified by Kugel-Rohr distillation to afford a yellow oil that solidified upon standing.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07378427B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-87976d20776a4b68900d43557a124f07 |
| Source note | uspto-grants-2008_05 |