HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophenol → 3-Fluoro-2-phenylthio-5-trifluoromethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | 2,3-Difluoro-5-(trifluoromethyl)pyridine | HCID 13421547 | — |
| Catalyst | Copper | HCID 23978 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Fluoro-2-phenylthio-5-trifluoromethylpyridine | HCID 18466518 | — |
Reaction Conditions
| Temperature | 160 °C |
|---|
Reaction Steps
Over a period of 2.5 h, 59.6 g (0.326 mol) of 2,3-difluoro-5-trifluoromethylpyridine were added at 148-156° C. to 37.7 g (0.338 mol) of 98.7% pure thiophenol and 2.1 mg (0.01 mol %) of copper powder, and the mixture was stirred at 156-164° C. for 2 hours. After cooling, the residue was taken up in methylene chloride, washed with 0.5 N of aqueous sodium hydroxide solution and with water, dried over magnesium sulfate and concentrated under reduced pressure. 88.9 g (100% of theory) of the title compound of n24/D=1.5539 were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06420314B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-1318a437b8b648be8b3e5dd013d7ff0b |
| Source note | uspto-grants-2002_07 |