反応式
[Cl:1][C:2]1[CH:8]=[C:7]([O:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:5][C:3]=1[NH2:4].ClC(Cl)(O[C:28](=[O:34])OC(Cl)(Cl)Cl)Cl.[CH2:36]([NH2:39])[CH2:37][CH3:38].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[Cl:1][C:2]1[CH:8]=[C:7]([O:9][C:10]2[C:19]3[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:5][C:3]=1[NH:4][C:28]([NH:39][CH2:36][CH2:37][CH3:38])=[O:34]参加物
実験手順
2-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]-aniline (5.13 g) was dissolved in chloroform (100 ml) and triethylamine (50 ml), and a solution of triphosgene (4.59 g) in chloroform (3 ml) was then added to the solution. The mixture was stirred for 30 min. Next, n-propylamine (2.74 g) was added to the reaction solution, and the mixture was stirred for additional 2 hr. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, and 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 chromatography on silica gel by development with chloroform/methanol (50/1) to give 4.14 g (yield 64%) of the title compound.
後処理
- stirringthe mixture was stirred for additional 2 hr
- 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 chromatography on silica gel by development with chloroform/methanol (50/1)
出典と根拠
- ORDレコード
- ord-887ef81314a145d6a5c11a88b324e54c
- 出典データセット
- uspto-grants-2007_01
- 特許番号
- US07169789B2
関連ノート
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