関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | 2,6-Dibromo-3-nitropyridin-4-amine | HCID 53249765 | — |
| 生成物 | 2,6-Dibromo-4-chloro-3-nitropyridine | HCID 58948143 | — |
反応手順
2,6-Dibromo-4-amino-5-nitro-pyridine (3 g) was taken up in concentrated hydrochloric acid (20 mL) and cooled to 0° C. Sodium nitrite (3.5 g) was added and the reaction mixture was allowed to stir at 0° C. for 1 h. The ice bath was removed and the reaction allowed to warm to room temperature over 3 h, and was then quenched by the addition of ethyl acetate (50 mL) and water (100 mL). The organic layer was separated, dried over MgSO4 and filtered and evaporated in vacuo to a pale yellow oil, which was purified by column chromatography using 35:1 pentane:EtOAc as eluant to give the title compound (2.2 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07691877B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-8f145f331fea473dbe193015c2f9acc9 |
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| 出典メモ | uspto-grants-2010_04 |
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