関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 2-Bromo-5-fluoro-3-nitropyridine | HCID 20791243 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Bromo-5-fluoropyridin-3-amine | HCID 40427367 | 81.2% |
反応手順
A suspension of 2-bromo-5-fluoro-3-nitropyridine (4.42 g, 20 mmol) and SnCl2 (22.56 g, 100 mmol) in EtOH (40 mL) and concentrated HCl (40 mL) was heated at 60° C. for 1 h. The reaction mixture was concentrated under reduced pressure. To the residue was added EtOAc (100 mL) and sat'd aq. NaHCO3 solution (200 mL), and the mixture was filtered with Celite® and extracted with EtOAc (100 mL×3). The organic layer was washed with saturated NaHCO3, water and brine, dried (MgSO4), filtered, and concentrated under reduced pressure to afford 3.1 g (80%) of 2-bromo-5-fluoropyridin-3-amine as a brown solid. MS (ESI): m/z=191.1 [M+1]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08815877B2 |
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| 出典データセット | uspto-grants-2014_08 |
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| ORD ID | ord-f9fefd6e1f4e4c79b7cca736daa2e513 |
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| 出典メモ | uspto-grants-2014_08 |
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