関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,5-Dichloro-2,4,6-trifluoropyridine | HCID 61273 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,5-Dichloro-2-fluoro-4,6-bis(2,2,2-trifluoroethoxy)pyridine | HCID 18544801 | — |
反応手順
A reaction flask was loaded with 3,5-dichloro-2,4,6-trifluoropyridine (5.6 g), DMF (15 ml), and potassium carbonate (9.2 g), and heated up to 30° C. with stirring. To this, a mixture of 2,2,2-trifluoroethanol (5.6 g) and DMF (10 ml) was dropwise added in one hour. After the dropwise addition was ended, the temperature was raised to 50° C., followed by stirring for three hours. The heating was stopped and left to cool. Thereafter, water (100 ml) was added to the reaction mixture, followed by extraction with ether. The ether layer was condensed to give 3,5-dichloro-2-fluoro-4,6-bis(2,2,2-trifluoroethoxy)pyridine (9.7 g). By GC/MS analysis, a molecular ion peak of 362 was confirmed.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06551682B1 |
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| 出典データセット | uspto-grants-2003_04 |
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| ORD ID | ord-739964c9f58f41cd846ebea9cf3e870e |
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| 出典メモ | uspto-grants-2003_04 |
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