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HRID 23321作成日:2026年10月23日
2,2,3,3-Tetrafluoro-1-propanol → 2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxy-6-(2,2,3,3-tetrafluoropropyloxy)pyridine
https://huagongshe.com/ja/reaction/23321
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,3,3-Tetrafluoro-1-propanol | HCID 6441 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine | HCID 22572630 | — |
| 溶媒 | Sulfolane | HCID 31347 | — |
| 溶媒 | Ethyl acetate pentane | HCID 22335286 | — |
| 生成物 | 2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxy-6-(2,2,3,3-tetrafluoropropyloxy)pyridine | HCID 22572642 | 99.2% |
反応手順
To a mixture of 2,2,3,3-tetrafluoropropan-1-ol (0.29 g, 2.2 mmol) in dry sulfolane (2 ml) is added NaH (60% in oil, 0.09 g, 2.2 mmol) and 2,6-bis-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine (0.8 g, 1.8 mmol). After stirring at 110° C. for 3.7 h the mixture is cooled to ambient temperature. The resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed 10 times with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.72 g, 57% yield) of m.p. 73-74° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06852673B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-facc9139d28f472d8d74f9b9d1df1032 |
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| 出典メモ | uspto-grants-2005_02 |
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