関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3,4,5-Trichloronitrobenzene | HCID 88365 | — |
| 反応物 | Potassium phenoxide | HCID 23670670 | — |
| 溶媒 | Diethylene Glycol | HCID 8117 | — |
| 生成物 | 2,6-Dichloro-4-nitrophenol | HCID 12066 | — |
反応手順
3,4,5-Trichloronitrobenzene (14.86 g) is added to a solution of potassium phenoxide (8.66 g) in diethylene glycol (66 mL) and the mixture is heated to 160° C. for approximately 15 hours. The resulting dark brown solution is cooled to room temperature, poured onto 100 mL cold water, and extracted twice with diethyl ether. The pooled organic extracts are washed with water, 10% aqueous sodium hydroxide, and then dried over anhydrous magnesium sulfate. Following removal of the solvent under reduced pressure the resulting oil is distilled in a Kugelrohr apparatus to provide a yellow oil that solidifies on standing. Recrystallization from ethanol-water provides the desired product as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06271236B1 |
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| 出典データセット | uspto-grants-2001_08 |
|---|
| ORD ID | ord-5a54bdf57cc248419b539a2c0541f10d |
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| 出典メモ | uspto-grants-2001_08 |
|---|