Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl 2,4-dioxo-4-(pyridin-2-yl)butanoate → 5-Hydroxy-1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)-4,5-dihydropyrazole-3-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl 2,4-dioxo-4-(pyridin-2-yl)butanoate | HCID 12171345 | — |
| 반응물 | 5-Hydrazinyl-2-methoxypyridine | HCID 22217853 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 5-Hydroxy-1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)-4,5-dihydropyrazole-3-carboxylic acid ethyl ester | HCID 23143676 | — |
반응 단계
4-(2-Pyridyl)-2,4-dioxobutanoic acid ethyl ester (1.10 g) obtained from Referential Example 31 and 5-hydrazino-2-methoxypyridine (0.692 g) obtained from Referential Example 2 were dissolved in ethanol (22 mL). The resultant mixture was refluxed under heat for 14 hours, followed by cooling in air. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate), followed by purification through silica gel column chromatography (toluene-acetone), to thereby give 5-hydroxy-1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)-4,5-dihydropyrazole-3-carboxylic acid ethyl ester as a solid substance (0.575 g, 34%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07622471B2 |
| 출처 데이터셋 | uspto-grants-2009_11 |
| ORD ID | ord-170b13e042244dee9a638a215342bbcf |
| 출처 메모 | uspto-grants-2009_11 |