Dimethylformamide dimethyl acetal → 4-((1E)-2-(Dimethylamino)ethenyl)-3-pyridinecarbonitrile
반응식
[CH3:1][N:2]([CH:4](OC)OC)[CH3:3].[CH3:9][C:10]1[C:15]([C:16]#[N:17])=[CH:14][N:13]=[CH:12][CH:11]=1>CN(C=O)C>[CH3:1][N:2]([CH3:3])/[CH:4]=[CH:9]/[C:10]1[C:15]([C:16]#[N:17])=[CH:14][N:13]=[CH:12][CH:11]=1참가 물질
4
반응 조건
- 온도
- 35 °C
실험 절차
940 ml of DMF dimethyl acetal are added to a solution of 200 g of 4-methylnicotinonitrile in 940 g of DMF, and the mixture is heated under reflux at 120-110 for 3 days. The mixture is cooled to 35° C., poured into 10 liters of ice-water and cooled at 4° C. for 16 h. The precipitate is filtered off, washed with water and dried, giving 263 g of 4-((E)-2-dimethylaminovinyl)nicotinonitrile; M˜173.22 g/mol; M+H found 174, NMR corresponds.
후처리
- temperaturethe mixture is heated
- temperatureunder reflux at 120-110 for 3 days
- temperaturecooled at 4° C. for 16 h
- filtrationThe precipitate is filtered off
- washwashed with water
- customdried
출처 및 근거
- ORD 기록
- ord-9c93a404358743598e18c0b4a190c824
- 출처 데이터셋
- uspto-grants-2016_07
- 특허 번호
- US09382244B2
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