Hydrochloric Acid → [8-chloro-3-(2-chloro-4-methanesulfonylbenzyl)-4-difluoromethoxy-2-methylquinolin-5-yloxy]acetic Acid
反応式
C[O:2][C:3](=[O:34])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]2[C:7]=1[C:8]([O:30][CH:31]([F:33])[F:32])=[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([CH3:28])(=[O:27])=[O:26])=[CH:21][C:20]=1[Cl:29])[C:10]([CH3:17])=[N:11]2.CO.[OH-].[Li+].Cl>O.O1CCCC1>[Cl:16][C:13]1[CH:14]=[CH:15][C:6]([O:5][CH2:4][C:3]([OH:34])=[O:2])=[C:7]2[C:12]=1[N:11]=[C:10]([CH3:17])[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([CH3:28])(=[O:27])=[O:26])=[CH:21][C:20]=1[Cl:29])=[C:8]2[O:30][CH:31]([F:33])[F:32]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
A mixture of [8-chloro-3-(2-chloro-4-methanesulfonylbenzyl)-4-difluoromethoxy-2-methylquinolin-5-yloxy]acetic acid methyl ester (0.034 g), methanol (8.0 mL), tetrahydrofuran (8.0 mL), water (5.0 mL) and lithium hydroxide (0.027 μg) was stirred at room temperature for 1 hour. The solution was acidified by the addition of 1.0 M aqueous hydrochloric acid and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and the solvent removed under reduced pressure. Purification of the residue by preparative reverse-phase HPLC using a gradient of acetonitrile in water gave title compound as a yellow solid, 0.09 g.
後処理
- extractionextracted with ethyl acetate
- dry with materialThe combined extracts were dried over magnesium sulfate
- customthe solvent removed under reduced pressure
- customPurification of the residue by preparative reverse-phase
出典と根拠
- ORDレコード
- ord-a3d9cc9951df46a4836415361665137e
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07858640B2
反応ノート
読み込み中…