関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | 2-Chlororesorcinol | HCID 80331 | — |
| 溶媒 | Potassium Hydroxide | HCID 14797 | — |
| 生成物 | 2-Chloro-3-methoxyphenol | HCID 15581471 | 72% |
反応手順
To an aqueous solution (100 mL) of potassium hydroxide (11.0 g) was added 2-chlorobenzene-1,3-diol (22.8 g). Then, dimethyl sulfate (19.9 g) was slowly added to the reaction mixture while keeping the reaction mixture at 10° C. to 20° C., and the mixture was stirred at 100° C. for 2 days. The reaction mixture was acidified with 2N hydrochloric acid, and the mixture was extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/petroleum ether) to give the title compound (18.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09315458B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-60c19c208b704da8ac733c8b083c62bd |
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| 出典メモ | uspto-grants-2016_04 |
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