Hydrochloric Acid → 7-Methoxy-2-oxo-8-pentyloxy-1,2-dihydroquinoline-3-carboxylic acid
反応式
C[O:2][C:3]([C:5]1[C:6](=[O:23])[NH:7][C:8]2[C:13]([CH:14]=1)=[CH:12][CH:11]=[C:10]([O:15][CH3:16])[C:9]=2[O:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])=[O:4].[OH-].[Na+].Cl>CO.O>[CH3:16][O:15][C:10]1[C:9]([O:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])=[C:8]2[C:13]([CH:14]=[C:5]([C:3]([OH:4])=[O:2])[C:6](=[O:23])[NH:7]2)=[CH:12][CH:11]=1参加物
6
実験手順
7-Methoxy-2-oxo-8-pentyloxy-1,2-dihydroquinoline-3-carboxylic acid methyl ester (240 mg) obtained in Example 1-1 was dissolved in methanol (7 ml) and water (3 ml), to which sodium hydroxide (120 ml) was added, and the solution was stirred at room temperature for 1.5 hours. While the reaction vessel was cooled with ice, the solution was acidified with the addition of concentrated hydrochloric acid, and extracted with ethyl acetate (20 ml). The organic layer was dried over anhydrous sodium sulfate, filtered to remove the desiccating agent, and concentrated under reduced pressure to give the title compound (228 ml) (Table 6).
後処理
- temperatureWhile the reaction vessel was cooled with ice
- extractionextracted with ethyl acetate (20 ml)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- customto remove the desiccating agent
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-77cc9f170bbe40c6bf4fdcba4bc53428
- 出典データセット
- uspto-grants-2003_01
- 特許番号
- US06509352B1
反応ノート
読み込み中…