反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:16]2[CH2:21][CH2:20][N:19]([C:22]([CH:24]3[CH2:28][CH2:27][CH2:26][O:25]3)=[O:23])[CH2:18][CH2:17]2)[N:3]=1.[ClH:29]>CO>[ClH:29].[CH3:9][O-:12].[ClH:29].[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:16]2[CH2:21][CH2:20][N:19]([C:22]([CH:24]3[CH2:28][CH2:27][CH2:26][O:25]3)=[O:23])[CH2:18][CH2:17]2)[N:3]=1参加物
実験手順
A solution of hydrogen chloride in methanol was prepared by bubbling the gas through dry methanol for several minutes. 1-(4-Amino-6,7-dimethoxy-2-quinazolinyl)-4-(tetrahydro-2-furoyl)piperazine (1.2 g, 3.1 mmol) was placed in an Erlenmeyer flask, together with a magnetic stirring bar, and the methanolic solution of hydrogen chloride was added until the solid had completely dissolved (about 13 mL). After the resulting mixture had stood at about 25° C. for several minutes, a precipitate formed. The mixture was cooled in an ice bath for thirty minutes and the precipitated solid collected by filtration to yield 1.1 g (2.41 mmol, 77.8%) of 1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-(tetrahydro-2-furoyl)piperazine monohydrochloride methanolate.
後処理
- customby bubbling the gas through dry methanol for several minutes
- dissolutionhad completely dissolved (about 13 mL)
- waitAfter the resulting mixture had stood at about 25° C. for several minutes
- customa precipitate formed
- temperatureThe mixture was cooled in an ice bath for thirty minutes
- filtrationthe precipitated solid collected by filtration
出典と根拠
- ORDレコード
- ord-d3d3bb326fba4875ab2dbbc113d0b222
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05412095
関連ノート
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