関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,6-Trifluoropyridine | HCID 2783289 | — |
| 反応物 | HCID 178481859 | HCID 178481859 | — |
| 溶媒 | Diisopropyl Ether | HCID 7914 | — |
| 溶媒 | Sulfolane | HCID 31347 | — |
| 溶媒 | Ethyl acetate pentane | HCID 22335286 | — |
| 生成物 | 2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine | HCID 15869678 | 93% |
反応手順
A mixture of 4.8 g (36 mmol) 2,4,6-trifluoropyridine, 19.8 g (119 mmol) 5-hydroxy-1-methyl-3-trifluoromethylpyrazole and 18.1 g (131 mmol) potassium carbonate in 25 ml anhydrous sulfolane is stirred and heated to 80° C. over a period of 3 days. After cooling, the 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 and the organic layer is dried over magnesium sulfate. After removal of the solvents, the residue is washed with isopropyl ether and 19.1 g (93% yield) colorless crystals of melting point 130° C. are obtained.
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-fe12c4b6675946fe8455049849d267c1 |
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| 出典メモ | uspto-grants-2005_02 |
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