反応式
CN(C)C=O.[CH2:6]([O:13][C:14]1[CH:23]=[C:22]2[C:17]([C:18]([O:24][C:25]3[C:26](I)=[N:27][C:28]([CH3:31])=[CH:29][CH:30]=3)=[CH:19][CH:20]=[N:21]2)=[CH:16][C:15]=1[O:33][CH3:34])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C([Sn](CCCC)(CCCC)[C:40]1[S:41][CH:42]=[CH:43][N:44]=1)CCC>[Cu]=O.O>[CH2:6]([O:13][C:14]1[CH:23]=[C:22]2[C:17]([C:18]([O:24][C:25]3[C:26]([C:40]4[S:41][CH:42]=[CH:43][N:44]=4)=[N:27][C:28]([CH3:31])=[CH:29][CH:30]=3)=[CH:19][CH:20]=[N:21]2)=[CH:16][C:15]=1[O:33][CH3:34])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 100 °C
実験手順
N,N-Dimethylformamide (2 ml) was added to 7-benzyloxy-4-(2-iodo-6-methyl-pyridin-3-yloxy)-6-methoxyquinoline (100 mg), tetrakistriphenylphosphine palladium (23 mg), tri-n-butyl-(thiazol-2-yl)-tin (113 mg), and copper(II) oxide (32 mg) under an argon atmosphere, and the mixture was stirred at 100° C. overnight. The reaction solution was cooled to room temperature, water was then added thereto, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using hexane-acetone to give the title compound (43 mg, yield 46%).
後処理
- temperatureThe reaction solution was cooled to room temperature
- extractionthe mixture was extracted with ethyl acetate
- washThe ethyl acetate layer was then washed with water
- dry with materialwas dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customthe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-8197771968384500918644a8315bf92d
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560558B2
関連ノート
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