참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-Chloro-2,3-dimethyl-1-oxidopyridin-1-ium | HCID 9877446 | — |
| 반응물 | (2,2-Bis(fluoromethyl)-1,3-dioxan-5-yl)methanol | HCID 59792580 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 4-((2,2-Bis(fluoromethyl)-1,3-dioxan-5-yl)methoxy)-2,3-dimethylpyridine 1-oxide | HCID 59792492 | 60.6% |
반응 단계
To a dimethylsulfoxide (10 ml) solution of the (2,2-bis(fluoromethyl)-1,3-dioxan-5-yl)methanol (1.6 g, 8.98 mmol) obtained in the step (7a), sodium hydride, in oil (431 mg, 9.88 mmol as the content was regarded as 55%) was added at room temperature. To the mixture, 4-chloro-2,3-dimethylpyridine 1-oxide (1.42 g, 8.98 mmol) was added and the mixture was stirred at 60° C. for 2 hours. After the reaction mixture was cooled to room temperature, it was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/methanol) to obtain the title compound (1.63 g, yield: 60.6%) as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07425634B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-9212ce16c1ab41cd8b73cacabfbfdd81 |
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| 출처 메모 | uspto-grants-2008_09 |
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