참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,4,6-Trifluoropyridine | HCID 2783289 | — |
| 반응물 | HCID 178481859 | HCID 178481859 | — |
| 용매 | Diisopropyl Ether | HCID 7914 | — |
| 용매 | Sulfolane | HCID 31347 | — |
| 용매 | Ethyl acetate pentane | HCID 22335286 | — |
| 생성물 | 2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine | HCID 15869678 | 93% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06852673B2 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-fe12c4b6675946fe8455049849d267c1 |
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| 출처 메모 | uspto-grants-2005_02 |
|---|