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Potassium Carbonate → 3-Bromo-2-ethynyl-5-(trifluoromethyl)benzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-5-(trifluoromethyl)-2-[(trimethylsilyl)ethynyl]aniline | HCID 57546201 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Bromo-2-ethynyl-5-(trifluoromethyl)benzenamine | HCID 57546030 | 73.6% |
反応手順
To a solution of 3-bromo-5-(trifluoromethyl)-2-((trimethylsilyl)ethynyl)aniline (2.70 g) in methanol (30 mL) was added potassium carbonate (1.11 g), and the mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, to the residue was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous ammonium chloride solution and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.56 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09296746B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-d500e91c93514259ac59da004a617a7a |
| 出典メモ | uspto-grants-2016_03 |