HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 1-(5-Bromo-4-methylpyridin-2-yl)-2,2,2-trifluoroethane-1,1-diol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | 1-(5-Bromo-4-methylpyridin-2-yl)-2,2,2-trifluoroethanol | HCID 67974798 | — |
| Product | 1-(5-Bromo-4-methylpyridin-2-yl)-2,2,2-trifluoroethane-1,1-diol | HCID 71115050 | — |
Reaction Steps
To a solution of 1-(5-bromo-4-methylpyridin-2-yl)-2,2,2-trifluoro-ethanol (345 mg; 1.2775 mmol) in dichloromethane (10 mL; 156.0 mmol) was added Dess-Martin periodinane (0.7313 g; 1.672 mmol). The reaction mixture was stirred at room temperature for 5 hours. 20 mL of a 10% aqueous solution of sodium thiosulfate was added and the reaction stirred for an additional 10 minutes. The reaction mixture was washed with 2 M aqueous sodium carbonate, dried over MgSO4, filtered, and concentrated. The crude product was carried forward without purification. LCMS (ESI): M+H=286.0; 1H NMR (400 MHz, DMSO) δ 8.70 (s, 1H), 7.72 (s, 1H), 7.59 (s, 2H), 2.43 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08623889B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-4a90361ccab0431bb280ae68c5c6ccdf |
| Source note | uspto-grants-2014_01 |