Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4,4,4-Trifluoro-1-(3-methyl-4-methoxylphenyl)-1,3-butanedione → 5-Methanesulfonyl-2-[5-(4-methoxy-3-methyl-phenyl)-3-trifluoromethyl-pyrazol-1-yl]-pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4,4,4-Trifluoro-1-(3-methyl-4-methoxylphenyl)-1,3-butanedione | HCID 11391298 | — |
| 반응물 | 2-Hydrazino-5-(methylsulfonyl)pyridine hydrochloride | HCID 22226813 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 5-Methanesulfonyl-2-[5-(4-methoxy-3-methyl-phenyl)-3-trifluoromethyl-pyrazol-1-yl]-pyridine | HCID 12972729 | 43.3% |
반응 단계
4,4,4-Trifluoro-1-(3-methyl-4-methoxylphenyl)-1,3-butanedione (0.78 g, 3 mmol) and 2-hydrazino-5-(methylsulfonyl)pyridine hydrochloride (0.671 g, 3 mmol) were mixed in ethanol (60 ml), and the resulting reaction mixture was heated at reflux temperature for 72 hours. The reaction mixture was then cooled to room temperature, and the solvent was removed in vacuo. The residue was dissolved in EtOAc (250 ml), and the organic layer was washed with saturated NaHCO3 solution, brine, dried (MgSO4), and concentrated in vacuo. The residue was purified first by flash chromatography using 40% hexane in methylene chloride to and then by recrystallization from 3:1 of isooctane:methylene chloride to give the title compound (535 mg, 43%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06531492B1 |
| 출처 데이터셋 | uspto-grants-2003_03 |
| ORD ID | ord-409230996d9342e8a538fcfe41357dc6 |
| 출처 메모 | uspto-grants-2003_03 |