참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 반응물 | Pyridine, 4-chloro-3-methoxy-2-methyl-, 1-oxide | HCID 5083929 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Pyridine, 3-methoxy-2-methyl-4-(2,2,2-trifluoroethoxy)-, 1-oxide | HCID 14402953 | — |
반응 단계
6.7 g of potassium tert-butoxide were added in portions, at -20° C., while stirring and under a nitrogen atmosphere, 5 to 20 ml of trifluoroethanol. After the mixture had been warmed to 0° C., 5.2 g (30 mmol) of 2-methyl-3-methoxy-4-chloropyridine N-oxide were added in portions. The mixture was heated under reflux for 3 hours, and then left to cool down to room temperature; a further 3.45 g of potassium tert-butoxide were then added and the mixture was heated under reflux for 2 hours. After it had cooled down, 40 ml of water were added to the reaction mixture, which was then extracted with dichloromethane; the extract was then dried over MgSO4 and freed from the solvent in vacuo. The resulting oily product was subjected to further reaction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05658933 |
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| 출처 데이터셋 | uspto-grants-1997_08 |
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| ORD ID | ord-6da0327bc5974c779ac08df838b8c9f5 |
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| 출처 메모 | uspto-grants-1997_08 |
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