関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Bromo-2,6-dimethylanisole | HCID 278654 | — |
| 生成物 | 4(4-Chloro-3,5-dimethyl-phenoxy)-2,6-dimethylanisole | HCID 12767810 | — |
反応手順
A mixture of 94 g of 4-chloro-3,5-dimethyl-phenol, 129 g of 4-bromo-2,6-dimethyl-anisole, 40 g of potassium hydroxide and 5 g of copper powder was slowly heated to 180°-190° C. During this operation, first the corresponding potassium phenolate formed, and the water formed separated by distillation with a small amount of 4-bromo-2,6-dimethylanisole. At about 200°-220° C., further reaction yielding phenoxy-anisole took place. After about 4 to 5 hours, the reaction was complete. The cooled substance was extracted to exhaustion with a solvent which is not miscible with water, such as methylene chloride. The filtrate of inorganic salts formed was then shaken several times with 2 N sodium hydroxide solution and water. After vaporization of methylene chloride a crude product was obtained which was still contaminated by 4-bromo-2,6-dimethyl-anisole. After distillation, 86 g of 4(4-chloro-3,5-dimethyl-phenoxy)-2,6-dimethyl-anisole were obtained, boiling point: 186° C. under a pressure of 3 mm mercury.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04391995 |
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| 出典データセット | uspto-grants-1983_07 |
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| ORD ID | ord-cff8674d290f453d9095e3cc277f9a2d |
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| 出典メモ | uspto-grants-1983_07 |
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