반응식
[NH:1]1[CH:5]=[C:4]([C:6]2[C:7]3[CH:14]=[CH:13][N:12](COCC[Si](C)(C)C)[C:8]=3[N:9]=[CH:10][N:11]=2)[CH:3]=[N:2]1.C(#N)C.[C:26](#[N:31])[CH:27]=[C:28]([CH3:30])[CH3:29].C1CCN2C(=NCCC2)CC1>>[CH3:29][C:28]([N:2]1[CH:3]=[C:4]([C:6]2[C:7]3[CH:14]=[CH:13][NH:12][C:8]=3[N:9]=[CH:10][N:11]=2)[CH:5]=[N:1]1)([CH3:30])[CH2:27][C:26]#[N:31]참가 물질
5
반응 조건
- 온도
- 60 °C
실험 절차
To a solution of 4-(1H-pyrazol-4-yl)-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]-pyrimidine (0.216 g, 0.684 mmol) in ACN (4 mL, 0.08 mol) was added crude senecionitrile (0.111 g, 1.37 mmol), followed by DBU (200 μL, 0.002 mol) and the resulting mixture was heated to 60° C. for 23 hours. The mixture was cooled to room temperature and the ACN was evaporated. The mixture was diluted with ethyl acetate and washed with dilute HCl and brine. The organic solution was dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (ethyl acetate/hexanes) afforded the desired product.
후처리
- temperatureThe mixture was cooled to room temperature
- customthe ACN was evaporated
- additionThe mixture was diluted with ethyl acetate
- washwashed with dilute HCl and brine
- dry with materialThe organic solution was dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customPurification by silica gel chromatography (ethyl acetate/hexanes)
출처 및 근거
- ORD 기록
- ord-170cbb614b3344288473e0c2b2879096
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08530485B2
연결된 노트
불러오는 중…