関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3,5,6-Tetrafluorophenol | HCID 69858 | — |
| 反応物 | 2-Chloro-5-nitrobenzonitrile | HCID 85504 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(2,3,5,6-Tetrafluorophenoxy)-5-nitrobenzonitrile | HCID 9106965 | 73% |
反応手順
In a 250 ml single-neck flask equipped with a magnetic stirrer and a reflux condenser fitted with a nitrogen bubbler were placed 9.13 g (0.050 moles) of 2-chloro-5-nitrobenzonitrile, 8.55 (0.0515 moles) of 2,3,5,6-tetrafluorophenol, 7.10 g (0.0515 moles) of anhydrous K2CO3, and 75 ml of acetonitrile. The mixture was heated to reflux and held there for 3 hrs. The reaction mixture was then cooled to room temperature and diluted with 150 ml of deionized water. The product separated as a solid. The solid was filtered off, washed thoroughly with water, and air-dried. The air-dried solid was recrystallized from 300 ml of absolute ethanol to give 11.36 g (73% yield) of purified 2-(2,3,5,6-tetrafluorophenoxy)-5-nitrobenzonitrile, mp 152.5°-154.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04332820 |
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| 出典データセット | uspto-grants-1982_06 |
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| ORD ID | ord-7811d4ec5a884a558dd318a4f305640a |
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| 出典メモ | uspto-grants-1982_06 |
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