関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Chloroanthraquinone | HCID 6709 | — |
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | 4-Aminophenethyl alcohol | HCID 66904 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 触媒 | Cupric acetate | HCID 8895 | — |
| 生成物 | 1-[4-[2-Hydroxyethyl]phenyl]aminoanthraquinone | HCID 9928042 | — |
反応手順
HEPAAQ was prepared by a procedure described in Lord, M. W.; Peters, A. T.; J. Chem. Soc., Perkins Trans., 1,(20)2305-8, incorporated herein by reference, with a slight modification. In a 250 mL single-necked round-bottom flask equipped with a reflux condenser was placed 1-chloroanthraquinone (10.5 g), 4-aminophenethyl alcohol (11.2 g), potassium acetate (7.87 g), copper acetate (0.46 g), and nitrobenzene (75 mL). The flask was flushed with nitrogen and then heated to reflux for about 2 hours. The resulting mixture was filtered. The solvent was removed from the filtrate, and the resultant solid was washed with methanol. The product was purified by dissolving the dried filtrate in dichloromethane and chromatographing on a silica column using a 10/90 (v/v) acetone/dichloromethane mixture as the eluent. The solvent was removed from the chromatographed material and dried in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05663024 |
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| 出典データセット | uspto-grants-1997_09 |
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| ORD ID | ord-a6c7097116574a729bb00fdf365e2316 |
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| 出典メモ | uspto-grants-1997_09 |
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