반응식
Br[C:2]1[CH:3]=[N:4][C:5]([C:8]#[N:9])=N[CH:7]=1.[C:10](=O)([O-])[O-].[Cs+].[Cs+].[F:16][C:17]1[CH:39]=[CH:38][CH:37]=[CH:36][C:18]=1[O:19][C:20]1[C:34]([OH:35])=[CH:33][C:23]2[NH:24][C:25]([C:27]3[CH:32]=[N:31][CH:30]=[CH:29][N:28]=3)=[N:26][C:22]=2[CH:21]=1>CN1CCCC1=O>[F:16][C:17]1[CH:39]=[CH:38][CH:37]=[CH:36][C:18]=1[O:19][C:20]1[C:34]([O:35][C:2]2[CH:7]=[CH:10][C:5]([C:8]#[N:9])=[N:4][CH:3]=2)=[CH:33][C:23]2[NH:24][C:25]([C:27]3[CH:32]=[N:31][CH:30]=[CH:29][N:28]=3)=[N:26][C:22]=2[CH:21]=1참가 물질
5
반응 조건
- 온도
- 90 °C
실험 절차
7.0 mg of 5-bromo-2-cyano-pyrimidine and 15 mg of cesium carbonate were added to an N-methylpyrrolidinone (0.5 ml) solution of 7.0 mg of 5-(2-fluorophenoxy)-6-hydroxy-2-pyrazin-2-yl-1H-benzimidazole obtained in the step 1, and the reaction liquid was stirred at 90° C. for 15 minutes. The reaction mixture was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]. The resulting fraction was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound a colorless solid.
후처리
- customobtained in the step 1
- customthe reaction liquid
- customThe reaction mixture was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]
- additionThe resulting fraction was diluted with ethyl acetate
- washwashed with aqueous saturated sodium bicarbonate
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated away under reduced pressure
- customto obtain the entitled compound a colorless solid
출처 및 근거
- ORD 기록
- ord-16448ad5041148a9ab574d8ff2b42526
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07728025B2
연결된 노트
불러오는 중…