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Sodium Thiosulfate → 4-Bromo-2-fluoro-3,5-dimethylphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| 反応物 | Pyridinium, 1-fluoro-, 1,1,1-trifluoromethanesulfonate (1:1) | HCID 2724576 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 4-Bromo-2-fluoro-3,5-dimethylphenol | HCID 59342598 | 36.2% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732626B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-cbdc6c6d5028454a97a4fb8644a9ff86 |
| 出典メモ | uspto-grants-2010_06 |