Water → 1-(3-Fluorophenyl)-4-oxocyclohexanecarbonitrile
반응식
[C:1]([C:3]1([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH:5](C(OC)=O)[CH2:4]1)#[N:2].O>CS(C)=O>[C:1]([C:3]1([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1)#[N:2]참가 물질
4
반응 조건
- 온도
- 150 °C
실험 절차
A mixture of 1-cyano-1-(3-fluorophenyl)-3-methoxycarbonylcyclohexan-4-one (57, 51 g, 185 mmol), water (54.8 mL) and DMSO (840 mL) was heated and stirred at 150° C. for 3 hours, followed by stirring at room temperature overnight. The reaction mixture was evaporated and purified by chromatography on silica gel. Elution with ethyl acetate/heptane (5%:95% to 30%:70%) gave 28 g of desired material as a solid product. Rt=3.89 min (Method 3). Detected mass: 218.2 (M+H+).
후처리
- temperaturewas heated
- stirringby stirring at room temperature overnight
- customThe reaction mixture was evaporated
- custompurified by chromatography on silica gel
- washElution with ethyl acetate/heptane (5%:95% to 30%:70%)
출처 및 근거
- ORD 기록
- ord-c826da8d534e40158cc0e144bb4304b5
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08541449B2
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