反応式
[SH:1][CH2:2][CH2:3][OH:4].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[C:16]([N:19]1[CH2:23][CH2:22][CH2:21][CH:20]1[C:24]1[C:25]([O:39][C:40]2[CH:41]=[N:42][C:43](Cl)=[CH:44][CH:45]=2)=[CH:26][C:27]2[N:31]=[C:30]([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=3)[NH:29][C:28]=2[CH:38]=1)(=[O:18])[CH3:17]>C(=O)(O)[O-].[Na+]>[C:16]([N:19]1[CH2:23][CH2:22][CH2:21][CH:20]1[C:24]1[C:25]([O:39][C:40]2[CH:45]=[CH:44][C:43]([S:1][CH2:2][CH2:3][OH:4])=[N:42][CH:41]=2)=[CH:26][C:27]2[N:31]=[C:30]([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=3)[NH:29][C:28]=2[CH:38]=1)(=[O:18])[CH3:17]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 120 °C
実験手順
20 mg of 2-mercaptoethanol and 10 mg of potassium carbonate were added in order to an N,N-dimethylformamide (1 ml) solution of 20 mg of 6-(1-acetylpyrrolidin-2-yl)-5-(6-chloropyridin-3-yl)oxy-2-pyridin-2-yl-1H-benzimidazole obtained in Example 504, and the reaction liquid was stirred at 120° C. for 5 hours. After cooled, the reaction liquid was diluted with aqueous saturated sodium bicarbonate, extracted with chloroform, and the organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated away under reduced pressure. The resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1) to obtain the entitled compound as a white solid.
後処理
- customthe reaction liquid
- temperatureAfter cooled
- customthe reaction liquid
- extractionextracted with chloroform
- dry with materialthe organic layer was dried with anhydrous magnesium sulfate
- customthe solvent was evaporated away under reduced pressure
- customThe resulting residue was purified
- customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1)
出典と根拠
- ORDレコード
- ord-789f003969094e3887548f5c03ce85d9
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728025B2
関連ノート
読み込み中…