Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trifluoroiodomethane | HCID 16843 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178503086 | HCID 178503086 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18929397 | HCID 18929397 | — |
Reaction Steps
Sodium hydride was added dropwise to a suspension of 0.5 g of 3-(2,6-dichloro-4-trifluoromethylphenyl)-5(methylsulfenyl)pyrazole (compound 16) in 5 ml of anhydrous N,N-dimethylformamide at 0° C., and the mixture was stirred at room temperature. An excess of trifluoromethyl iodide was introduced into the reaction mixture, and the resulting mixture was stirred for 3 hours with the reactor closed. The reaction mixture was poured into water, followed by extraction with ether, washing with brine and drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain a residue, which was purified by column chromatography on silica gel (eluent: chloroform/hexane=1/20), giving 0.2 g of the desired product in the form of light brown oil (yield 33.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05739083 |
|---|
| Source dataset | uspto-grants-1998_04 |
|---|
| ORD ID | ord-08e0aa15fe0d4faca37fc8e68544b81c |
|---|
| Source note | uspto-grants-1998_04 |
|---|