関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 5-Nitro-2,3'-bipyridin-6-amine | HCID 20550367 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Bromo-5-nitro-2,3'-bipyridin-6-amine | HCID 59596002 | 100.7% |
反応手順
To a 0° C. cooled stirred solution of 5-nitro-2,3′-bipyridin-6-amine (4.8 g, 22.2 mmol) in DMF (50 mL), N-bromosuccinimide (4.75 g, 26.7 mmol) was added in portions. After stirring at room temperature for 16 h, the solvent was removed under reduced pressure. The crude residue was solved with ethyl acetate and washed with saturated potassium carbonate aqueous solution. The organic layer was washed with brine, dried (MgSO4) and evaporated. The residue was purified by silica gel flash chromatography (95:5 dichloromethane/methanol) to give the title compound (6.6 g, 100%) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07855202B2 |
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| 出典データセット | uspto-grants-2010_12 |
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| ORD ID | ord-599d982637a347b980b45430f25fa1f0 |
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| 出典メモ | uspto-grants-2010_12 |
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