反応式
C1COCC1.CO.[OH-].[Na+].[Cl:10][C:11]1[C:12]([NH:24][C:25]([C:27]2[C:35]3[C:30](=[CH:31][CH:32]=[C:33]([F:36])[CH:34]=3)[N:29]([CH3:37])[CH:28]=2)=[O:26])=[CH:13][C:14]([F:23])=[C:15]([CH2:17][C:18]([O:20]CC)=[O:19])[CH:16]=1>Cl>[Cl:10][C:11]1[C:12]([NH:24][C:25]([C:27]2[C:35]3[C:30](=[CH:31][CH:32]=[C:33]([F:36])[CH:34]=3)[N:29]([CH3:37])[CH:28]=2)=[O:26])=[CH:13][C:14]([F:23])=[C:15]([CH2:17][C:18]([OH:20])=[O:19])[CH:16]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
THF/methanol (1/1, 60 ml) and 0.25N NaOH (43 ml, 10.6 mmol) were added to ethyl (5-chloro-2-fluoro-4-(((5-fluoro-1-methyl-3-indolyl)carbonyl)amino)phenyl)acetate (865 mmol, 2.13 mmol) and the mixture was stirred at room temperature for 3 hours. The reaction mixture was poured in 1N HCl, followed by extraction with a chloroform/methanol (10/1) mixture. The extract was dried over anhydrous sodium sulfate, and distilled under reduced pressure to remove the solvent. The residue was solidified with methanol/chloroform/hexane. The crystals thus precipitated were collected by filtration under reduced pressure and dried under reduced pressure to give (5-chloro-2-fluoro-4-(((5-fluoro-1-methyl-3-indolyl)carbonyl)amino)phenyl)acetic acid (736 mg, 91%) as a white crystalline powder.
後処理
- extractionfollowed by extraction with a chloroform/methanol (10/1) mixture
- dry with materialThe extract was dried over anhydrous sodium sulfate
- distillationdistilled under reduced pressure
- customto remove the solvent
- customThe crystals thus precipitated
- filtrationwere collected by filtration under reduced pressure
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-d34fa89d6d9a42f9932a5d19f62f30cb
- 出典データセット
- uspto-grants-2007_01
- 特許番号
- US07157487B2
関連ノート
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