関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | 1-Chloro-4-hydroxyanthraquinone | HCID 66510 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 触媒 | Cupric acetate | HCID 8895 | — |
| 生成物 | (+)-1-[p-(4-Methylhexyl)anilino]-4-hydroxyanthraquinone | HCID 20494911 | — |
反応手順
1-Chloro-4-hydroxyanthraquinone (27.8 gm) is dissolved in 200 ml nitrobenzene in a boiling flask fitted with a stirrer and reflux condensor. After heating to 80° C., 18.1 gm (+)-4-methylhexyl)aniline, prepared according to Example 17, is added followed by the addition of 0.1 gm copper acetate and 20 gm sodium acetate. The mixture is stirred and heated to 150° C. for 4 hours. The mixture is then cooled to 80° C. and 500 ml ethanol is added. When cooled to room temperature the crude dye is separated by filtration, water and alcohol washed, and dried overnight. Chromatography on alumina using toluene as eluent affords the pure helichromic compound. The structure of the compound is confirmed by NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04394070 |
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| 出典データセット | uspto-grants-1983_07 |
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| ORD ID | ord-5a552999306f466fa173de75f13ffa87 |
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| 出典メモ | uspto-grants-1983_07 |
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