関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | 2-Amino-5-fluorobenzonitrile | HCID 2737704 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Amino-3-chloro-5-fluorobenzonitrile | HCID 66801728 | 100% |
反応手順
To a solution of 2-amino-5-fluorobenzonitrile (9.90 g, 72.8 mmol) in acetonitrile (200 mL) was added N-chlorosuccinimide (10.7 g, 80.1 mmol) in several portions. The reaction mixture was heated at 80° C. for 16 hours, then cooled and concentrated to approximately 100 mL under reduced pressure. The residue was poured into water (1 L), and the resultant precipitate was filtered, washed with water and dried (50° C. under vacuum) to give the title compound as a light brown solid (12.37 g, 100%). 1H NMR (300 MHz, CDCl3): δ 7.27 (dd, J=7.9, 2.9 Hz, 1H), 7.09 (dd, J=7.9, 2.9 Hz, 1H), 4.69 (br s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08697708B2 |
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| 出典データセット | uspto-grants-2014_04 |
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| ORD ID | ord-b60f57cc6c3c4217a1e9ec18fe3d0cd3 |
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| 出典メモ | uspto-grants-2014_04 |
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