2-Propanone, methylhydrazone → 3-((1-Methyl-2-(propan-2-ylidene)hydrazinyl)methylene)pentane-2,4-dione
반응식
C(O[CH:4]=[C:5]([C:9](=[O:11])[CH3:10])[C:6](=[O:8])[CH3:7])C.[CH3:12][NH:13][N:14]=[C:15]([CH3:17])[CH3:16]>CCOCC>[CH3:12][N:13]([CH:4]=[C:5]([C:6](=[O:8])[CH3:7])[C:9](=[O:11])[CH3:10])[N:14]=[C:15]([CH3:17])[CH3:16]참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
3-(ethoxymethylene)pentane-2,4-dione (Preparation 2, 8.6 g) was dissolved in Ether (30 mL) and cooled to 0° C. The reaction solution was then slowly treated with 1-methyl-2-(propan-2-ylidene)hydrazine (Preparation 1, 4.8 g) dropwise over 5 minutes, and then warmed and stirred at room temperature overnight. The reaction solution was purified directly by flash column chromatography (Biotage Quad 25; Eluent: 20% EtOH in EtOAc) to afford the title compound as a light red solid. (9.1 g, 84.0%).
후처리
- temperaturewarmed
- customThe reaction solution was purified directly by flash column chromatography (Biotage Quad 25; Eluent: 20% EtOH in EtOAc)
출처 및 근거
- ORD 기록
- ord-9d8001702bc04b4d93640fec5a09ac87
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09446046B2
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