関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,3-Dichloro-5-(trifluoromethyl)pyridine | HCID 112234 | — |
| 反応物 | 2-(Pyridin-2-YL)acetaldehyde | HCID 11715172 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-Chloro-5-(trifluoromethyl)pyridine | HCID 2736698 | 7.1% |
反応手順
Add zinc dust (1.18 g) to a suspension of 2,3-dichloro-5-trifluoromethyl-pyridine (2.0 g, 9.30 mmol) in 80:20 water and acetic acid (5 mL) and stir at 90° C. for 1 h. Add more zinc dust (1g) and stir at 90° C. for an additional 15 min. Cool the reaction mixture to room temperature, filter, and wash with dichloromethane. Carefully concentrate and purify the residue by silica gel chromatography, eluting with 100:0 to 0:100 hexane:dichloromethane, to obtain the title compound as a volatile oil (0.120g, 7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07915424B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-a90e4a127c254a10a0cebcff8276d27e |
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| 出典メモ | uspto-grants-2011_03 |
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