Dimethylformamide → HCID 9953325, 화합물
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[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]=1참가 물질
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-9c6d1a5364cb41ae89eda5e62a6faea6
- 출처 데이터셋
- uspto-grants-2003_01
- 특허 번호
- US06509352B1
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