HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → 4-Bromo-2-fluoro-3,5-dimethylphenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| Reactant | Pyridinium, 1-fluoro-, 1,1,1-trifluoromethanesulfonate (1:1) | HCID 2724576 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | 4-Bromo-2-fluoro-3,5-dimethylphenol | HCID 59342598 | 36.2% |
Reaction Steps
To a solution of 4-bromo-3,5-dimethylphenol (2.00 g, 9.95 mmol) in 1,2-dichloroethane (20 mL) was added N-fluoropyridinium triflate (6.15 g, 24.9 mmol), and the mixture was heated under reflux for 7 hr. The reaction mixture was treated with 1 M aqueous sodium thiosulfate solution, and extracted with ethyl acetate. The extract was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=0:100-30:70) to give the title compound (0.790 g, yield 36%) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08492430B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-c6b0ce29acba4d0199cd8c36bc85c3b6 |
| Source note | uspto-grants-2013_07 |