反応式
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=3)[N:12]=[CH:11][N:10]=2)[CH:5]=[CH:4][C:3]=1[NH:23][C:24]([NH:26][CH2:27][CH2:28][CH3:29])=[O:25].[H-].[Na+].[C:32](Cl)(=[O:34])[CH3:33]>O1CCCC1>[C:32]([N:23]([C:3]1[CH:4]=[CH:5][C:6]([O:8][C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=3)[N:12]=[CH:11][N:10]=2)=[CH:7][C:2]=1[Cl:1])[C:24]([NH:26][CH2:27][CH2:28][CH3:29])=[O:25])(=[O:34])[CH3:33]参加物
実験手順
N-{2-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]-phenyl}-N′-propylurea 100 mg) was dissolved in anhydrous tetrahydrofuran (30 ml), and sodium hydride (60 wt %, 88 mg) was added to the solution. The mixture was stirred at room temperature for 15 min. Next, acetyl chloride (63 μl) was added to the reaction solution, and the mixture was stirred at room temperature for additional 2 hr. The solvent was removed by distillation under the reduced pressure, and water was added to the residue. The mixture was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by HPLC by development with chloroform/acetone to give 27 mg (yield 26%) of the title compound.
後処理
- stirringthe mixture was stirred at room temperature for additional 2 hr
- customThe solvent was removed by distillation under the reduced pressure, and water
- additionwas added to the residue
- extractionThe mixture was extracted with chloroform
- dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customThe residue was purified by HPLC by development with chloroform/acetone
出典と根拠
- ORDレコード
- ord-9271b39b3c8c4e4ea6291735aeac74d7
- 出典データセット
- uspto-grants-2007_01
- 特許番号
- US07169789B2
関連ノート
読み込み中…