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N-Iodosuccinimide → 3-Bromo-2-iodo-5-(trifluoromethyl)aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | 3-Bromo-5-(trifluoromethyl)aniline | HCID 2735880 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Bromo-2-iodo-5-(trifluoromethyl)aniline | HCID 57546142 | 68.3% |
反応手順
To a solution of 3-bromo-5-(trifluoromethyl)aniline (5.00 g) in acetic acid (40 mL) was added N-iodosuccinimide (5.16 g) at 0° C., and the mixture was stirred overnight at room temperature under nitrogen atmosphere. The reaction mixture was diluted with ethyl acetate, washed with 10% aqueous sodium thiosulfate solution, saturated aqueous sodium bicarbonate 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 (5.21 g). 1H NMR (300 MHz, CDCl3) δ 4.58 (2H, brs), 6.84 (1H, d, J=1.1 Hz), 7.23 (1H, d, J=1.1 Hz).
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-4742f0dfcf32470bad86ff75ea01a13b |
| 出典メモ | uspto-grants-2016_03 |