反応式
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]=1参加物
5
反応条件
- 温度
- 90 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-16448ad5041148a9ab574d8ff2b42526
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728025B2
関連ノート
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