HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11517731, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 11538670 | HCID 11538670 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 11517731 | HCID 11517731 | 95% |
Reaction Steps
An ice-cold solution of 4-[[2-(phenylthio)ethyl](2,2,2-trifluoroethyl)amino]-2-(trifluoromethyl)benzonitrile (0.056 g, 0.138 mmol) in MeOH (6 mL) was treated with a solution of oxone (0.255 g, 0.415 mmol) in water (3 mL) and stirred at rt. After 1.5 h, the mixture was partitioned between EtOAc and water. The organic phase was washed with water and brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by silica gel chromatography (5-50% EtOAc/hexanes gradient) and the product crystallized from CH2Cl2/hexanes to give the title compound as a white solid (0.057 g, 95% yield): MS (ES) m/z 437 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834063B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-acafe5bad6c441d1afa2d9fae6ba65f2 |
| Source note | uspto-grants-2010_11 |