関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | 2-Chloro-3-fluoropyridine | HCID 2782791 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 1-(3-Fluoro-2-pyridinyl)piperazine | HCID 134987 | 73% |
反応手順
The product of Example 28A (3.3 g, 0.025 mol) in n-butanol (150 mL) at 23° C. was treated with piperazine (21.5 g, 0.25 mol) and then reflux for 3 days. The reaction mixture was allowed to cool to 23° C. and concentrated under reduced pressure. The residue was slurried with water and ethyl acetate. The ethyl acetate solution was separarted, dried over Na2SO4, filtered, and the filtrate concentrated under reduced pressure to afford 3.3 g (73% yield) of the title compound. 1H NMR (500 MHz, DMSO-d6) δ 2.80 (m, 4H), 3.38 (m, 4H), 6.84 (m, 1H), 7.47 (m, 1H), 7.98 (m, 1H); MS (ESI) m/e 182 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07351828B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-2ceda9972d994b22a1657fce47af09a7 |
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| 出典メモ | uspto-grants-2008_04 |
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