関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanone, 1-(2-amino-4,5-dimethoxyphenyl)- | HCID 602085 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | HCID 178419049 | HCID 178419049 | 87.3% |
反応手順
The starting material, 4-hydroxy-6,7-dimethoxycinnoline was obtained by adding a solution of sodium nitrite (1.9 g, 27 mmol) to a solution of 2-amino-4,5-dimethoxyacetophenone (5 g, 0.025 mol) in acetic acid (90 ml) and sulphuric acid (15 ml) at a rate to maintain the temperature below 20° C. The mixture was heated at 80° C. for 90 minutes. After cooling and concentrating the solution to half its original volume, the residue was poured into ether (800 ml). The solid was collected by filtration and suspended in water (200 ml). After adjusting to pH7 with sodium hydroxide the solid was filtered, washed with water, methanol and methylene chloride to give 4-hydroxy-6,7-dimethoxycinnoline (4.5 g, 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087602B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-a0ab3c0fa52b4471a489048eafec37c1 |
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| 出典メモ | uspto-grants-2006_08 |
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