関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Amino-3-fluoropyridine | HCID 817122 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-N-(3-fluoro-pyridin-4-yl)-acetamide | HCID 59503759 | — |
反応手順
A solution of 3-fluoro-pyridin-4-ylamine (0.2 g) in dry dichloromethane (2 mL) under nitrogen at 0° C. was treated with triethylamine (0.28 mL) followed by slow addition of chloroacetyl chloride (0.16 mL). The reaction mixture was allowed to warm up to room temperature. After 2 h, the mixture was partitioned between dichloromethane and water The phases were separated and the aqueous layer was extracted with dichloromethane (×2). The combined organic layer was washed with brine, dried over sodium sulphate, filtered and concentrated to give the crude product which was purified by silica gel chromatography eluting with 0-100% EtOAc/cyclohexane. The relevant fractions were combined and evaporated to give the title compound (0.11 g) as a pink solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08329729B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-ae5256a72c1b4a959f450ab91dcab968 |
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| 出典メモ | uspto-grants-2012_12 |
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