참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | (2,2-Dimethyl-1,3-dioxan-5-yl)methanol | HCID 3584869 | — |
| 반응물 | 4-Chloro-2,3-dimethyl-1-oxidopyridin-1-ium | HCID 9877446 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | HCID 59792424 | HCID 59792424 | 74.8% |
반응 단계
To a dimethyl sulfoxide (30 ml) solution of the (2,2-dimethyl-1,3-dioxan-5-yl)methanol (3.27 g, 22.4 mmol) separately obtained in the same manner as in the step (11a) in example 11, sodium hydride, in oil (837 mg, 20.9 mmol as the content was regarded as 60%) was added at room temperature. The mixture was stirred at room temperature for 15 minutes in a nitrogen atmosphere. To the mixture, 4-chloro-2,3-dimethylpyridine 1-oxide (3.03 g, 19.2 mmol) was added, and the mixture was stirred at 60° C. for 3 hours and 20 minutes. After cooled to room temperature, the reaction mixture was concentrated. The residue was purified by silica gel column chromatography (NH silica gel: 250 g, elution solvent: ethyl acetate, ethyl acetate/methanol=10/1) to obtain the title compound (3.84 g, yield: 74.8%) as a pale brown solid.
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-a2314bfcbc4e4f7ebdba088014d30d99 |
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| 출처 메모 | uspto-grants-2008_09 |
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