関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Sulfite | HCID 25041 | — |
| 反応物 | 6-Bromo-2-naphthalenol | HCID 27144 | — |
| 溶媒 | Ammonia | HCID 222 | — |
| 生成物 | 2-Amino-6-bromonaphthalene | HCID 348404 | 33.5% |
反応手順
6-Bromo-2-naphthol (2.0 g, 9 mmol), ammonium sulfite (10.4 g, 90 mmol) and 10 mL of ammonia solution were sealed in a tube. The reaction mixture was heated at 190° C. for 24 hrs and allowed to cool to room temperature, the reaction mixture was extracted with EtOAc. HCl (10%) was added to the organic layer to give a precipitate. After filtration, the solid was dissolved in 10% of Na2CO3 and extracted with EtOAc, the organic layer was dried over Na2SO4. The solvent was removed under reduced pressure to give the product as yellow solid (0.67 g, 33%). MS [M++43]=265, LC-MS: tR=2.14 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07696227B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-741906717e49449988e584edb2308dd6 |
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| 出典メモ | uspto-grants-2010_04 |
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