関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 2-Bromo-5-fluorobenzotrifluoride | HCID 520983 | — |
| 反応物 | 4-(2-Aminopyridin-3-yl)phenol | HCID 66748477 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-{4-[4-Bromo-3-(trifluoromethyl)phenoxy]phenyl}pyridin-2-amine | HCID 66748677 | 69.2% |
反応手順
Tripotassium phosphate (3.42 g) was added to a mixture of 4-(2-aminopyridin-3-yl)phenol (1.00 g) and 1-bromo-4-fluoro-2-(trifluoromethyl)benzene (1.57 g) in DMSO (15 mL). The mixture was stirred at 140° C. under nitrogen for 7 hr. Water and EtOAc were added and the extracted organic layer was washed with brine. Silica-gel was added to the organic layer and the volatiles were removed in vacuo. The mixture supported on silica-gel was purified by column chromatography (NH-silica gel, eluted with EtOAc in hexane) and concentrated to give 3-{4-[4-bromo-3-(trifluoromethyl)phenoxy]phenyl}pyridin-2-amine (1.52 g) as orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08778934B2 |
|---|
| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-68e2fffb7ba0400babf43887a2b4b31a |
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| 出典メモ | uspto-grants-2014_07 |
|---|
