関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloro-1,1-diethoxyethane | HCID 12128 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1,3-Benzenediol, 5-chloro- | HCID 94554 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(2,2-Diethoxyethoxy)-5-chlorophenol | HCID 20396693 | — |
反応手順
The monosodium salt of 3-hydroxy-5-chlorophenol (0.05 mole) and dimethylformamide (75 ml) are charged under nitrogen gas into a glass reacton vessel equipped with a mechanical stirrer, thermometer and addition funnel. The mixture is stirred until dissolved, and 1-chloro-2,2-diethoxyethane (0.05 mole) is added dropwise over a period of about 20 minutes. After the addition is completed, the reaction mixture is heated at about 90° C. with stirring for a period of about 48 hours. After this time water (200 ml) is added, and the reaction mixture is neutralized with ammonium chloride. The reaction mixture is then extracted with chloroform, and the organic phase is separated from the aqueous phase. The organic phase is then stripped of solvent, leaving an oil. This oil is distilled under reduced pressure to yield the desired product 3-(2,2-diethoxyethoxy)-5-chlorophenol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04163112 |
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| 出典データセット | uspto-grants-1979_07 |
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| ORD ID | ord-cff4abb0350044009f83411aa805bcc4 |
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| 出典メモ | uspto-grants-1979_07 |
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