関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,5-Dimethylanisole | HCID 74350 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 生成物 | 4-Methylcatechol | HCID 9958 | 65.7% |
反応手順
To an ice-cold concentrated nitric acid (200 mL) was added slowly under stirring over a period of 20 minutes 2-methoxy-1,4-dimethylbenzene (25 g, 184 mmol). To this cold reaction mixture, sodium nitrite (38 g, 552 mmol) was added slowly in lots over a period of 1 h while maintaining the temperature below 2° C. The reaction mixture was stirred at between 0-5° C. for 5 h. The reaction mass was poured into ice-cold water (1000 mL), and the precipitated solid was filtered, washed with cold water (100 mL) and dried. The crude solid was crystallized from ethanol and water (7:1) to yield compound 1 (15 g, 45%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434724B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-7a72b8535733418f8997d35b7dd91617 |
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| 出典メモ | uspto-grants-2016_09 |
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