関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | p-(Trifluoromethoxy)phenol | HCID 70015 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Trifluoromethoxysalicylic acid | HCID 2775103 | — |
反応手順
178 g (1 mol) of 4-trifluoromethoxyphenol and 345 g (2.5 mol) of potassium carbonate were initially introduced into an autoclave which was then pressurized to 60 bar with carbon dioxide and heated at 200° C. for 4 hours. After cooling and releasing the pressure, the residue was dissolved in 1.5 l of hot water, the solution was filtered hot, the cooled filtrate was extracted using methylene chloride and the extract was clarified using active carbon. The pH was then adjusted to 1 and the precipitated product was filtered off with suction. 192 g of product having a melting point of 129° C. were obtained, which corresponds to 86% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04956370 |
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| 出典データセット | uspto-grants-1990_09 |
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| ORD ID | ord-753b479947974eae883af69265b3ba90 |
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| 出典メモ | uspto-grants-1990_09 |
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