HuagongsheHuagongshe Chemistry Print Report · For research reference only
Fluorine → HCID 18951399, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Fluorine | HCID 24524 | — |
| Reactant | HCID 18951398 | HCID 18951398 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 18951399 | HCID 18951399 | — |
Reaction Steps
To a mixture of 3-(trifluoromethyl)pyridine-2-sulfonic acid (115 mg, 0.5 mmol) and acetonitrile (20 ml) in a flask on a cooling bath kept at -10° C., a mixed gas of 10% fluorine/90% nitrogen was introduced at a flow rate of 15 ml/min. The total amount of the fluorine gas was 1.5 mmol. Thereafter, the nitrogen gas alone was introduced for 30 minutes. After the reaction mixture was concentrated, ethyl acetate was added to the residue. The precipitated crystal was recovered by filtration to obtain N-fluoro-3-(trifluoromethyl)pyridinium-2-sulfonate (84.6 mg, 0.345 mmol). Yield, 69%. Melting point, 180°-196° C. (with decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05374732 |
| Source dataset | uspto-grants-1994_12 |
| ORD ID | ord-2c5c18885be7472cb586cc9a1f60b050 |
| Source note | uspto-grants-1994_12 |