Dimethylformamide → HCID 9953325、化合物
反応式
[CH3:1][O:2][C:3]1[C:12]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[C:11]2[C:6]([CH:7]=[C:8]([C:20]([OH:22])=O)[C:9](=[O:19])[NH:10]2)=[CH:5][CH:4]=1.O.O[N:25]1[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33]C=2N=N1.C(O[CH2:38][CH3:39])(=O)C.C(=O)([O-])O.[Na+].C[N:46](C)C=O>>[N:46]1[CH:33]=[CH:32][C:31]([CH2:30][CH2:29][NH:25][C:20]([C:8]2[C:9](=[O:19])[NH:10][C:11]3[C:6]([CH:7]=2)=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[C:12]=3[O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[O:22])=[CH:39][CH:38]=1参加物
実験手順
7-Methoxy-2-oxo-8-pentyloxy-1,2-dihydroquinoline-3-carboxylic acid (30.0 mg) obtained in Example 2-1,2-pyridine-4-ylethylamine (36.0 mg), and 1-hydroxybenzotriazole hydrate (17.3 mg) were dissolved in dimethylformamide (2 ml), and 1-ethyl-3-(3-dimethyl-aminopropyl)carbodiimide hydrochloride (24.5 mg) was successively added to this solution while being cooled with ice. After the reaction solution was stirred at room temperature for 5 hours, ethyl acetate (3 ml) and a saturated aqueous solution of sodium hydrogencarbonate (3 ml) were added to this solution. The organic layer was separated and dried over anhydrous sodium sulfate, filtered to remove the desiccating agent, and concentrated under reduced pressure. The resultant residue was purified through column chromatography (eluent: a mixture of chloroform and methanol at a ratio of 25:1) to obtain the title compound (35 mg) as colorless crystals (Table 8).
後処理
- temperaturewhile being cooled with ice
- customThe organic layer was separated
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customto remove the desiccating agent
- concentrationconcentrated under reduced pressure
- customThe resultant residue was purified through column chromatography (eluent
- additiona mixture of chloroform and methanol at a ratio of 25:1)
出典と根拠
- ORDレコード
- ord-9c6d1a5364cb41ae89eda5e62a6faea6
- 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…