참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | N-Butyltriethylammoniumchloride | HCID 10888803 | — |
| 반응물 | Ethyl 2,4-dihydroxy-6-methylpyridine-3-carboxylate | HCID 54676534 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Ethyl 4-chloro-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylate | HCID 57859986 | 44% |
반응 단계
A mixture of ethyl 4-hydroxy-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylate (3.00 g, 15.2 mmol), phosphorus oxychloride (7.75 mL), n-butyltriethylammonium chloride (13.8 g, 60.8 mmol) and acetonitrile (60 mL) was stirred at 40° C. for 30 min and under refluxing conditions for 30 min. After cooling, the reaction mixture was concentrated under reduced pressure, water was added to the residue and the mixture was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was washed with ethyl acetate-hexane mixed solution, and dried under reduced pressure to give the title compound (1.45 g, 44%) as a white powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08217176B2 |
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| 출처 데이터셋 | uspto-grants-2012_07 |
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| ORD ID | ord-edd2d8dc3cc74ca1b023a46516c0b0b8 |
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| 출처 메모 | uspto-grants-2012_07 |
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