反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=O.[F:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][C:17]=1[F:18])[NH:14][C:13]([C:19]1[CH:20]=[CH:21][C:22]([O:26][CH3:27])=[C:23]([NH2:25])[CH:24]=1)=[CH:12]2.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[F:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][C:17]=1[F:18])[NH:14][C:13]([C:19]1[CH:20]=[CH:21][C:22]([O:26][CH3:27])=[C:23]([NH:25][CH2:6][C:2]3[S:1][CH:5]=[CH:4][CH:3]=3)[CH:24]=1)=[CH:12]2参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
2-Thiophenecarboxaldehyde (0.112 g, 1.0 mmol) was added to a stirred mixture of 5-(5,6-difluoro-1H-indol-2-yl)-2-methoxy-phenylamine (0.29 g, 1.06 mmol) in methylene chloride (125 mL), followed by acetic acid (0.1 g, 1.67 mmol). The resulting mixture was stirred at room temperature for 1 hour. Sodium triacetoxyborohydride (0.23 g, 1.09 mmol) was added in one portion, and the resulting homogeneous solution stirred at room temperature for 6 days. Saturated aqueous sodium bicarbonate solution (100 mL) was added and the mixture stirred for 2 hours. The mixture was shaken and the organic layer separated. The solvent was evaporated to give a brown gum. Recrystallization from methanol/water gave the product as a brown solid (120 mg), mp 190-192° C.
後処理
- stirringthe resulting homogeneous solution stirred at room temperature for 6 days
- stirringthe mixture stirred for 2 hours
- stirringThe mixture was shaken
- customthe organic layer separated
- customThe solvent was evaporated
- customto give a brown gum
- customRecrystallization from methanol/water
出典と根拠
- ORDレコード
- ord-adbbe9c4bdb14caca4ed935cc7bb7baf
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06858739B2
関連ノート
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