反応式
N(C(OCC)=O)=NC(OCC)=O.[Cl:13][C:14]1[CH:22]=[CH:21][C:17]2[CH:18]=[CH:19][O:20][C:16]=2[C:15]=1[NH:23][C:24]1[C:33]2[C:28](=[CH:29][C:30]([OH:36])=[C:31]([O:34][CH3:35])[CH:32]=2)[N:27]=[CH:26][N:25]=1.O[CH2:38][CH2:39][N:40]1[CH2:44][CH2:43][CH2:42][CH2:41]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Cl:13][C:14]1[CH:22]=[CH:21][C:17]2[CH:18]=[CH:19][O:20][C:16]=2[C:15]=1[NH:23][C:24]1[C:33]2[C:28](=[CH:29][C:30]([O:36][CH2:38][CH2:39][N:40]3[CH2:44][CH2:43][CH2:42][CH2:41]3)=[C:31]([O:34][CH3:35])[CH:32]=2)[N:27]=[CH:26][N:25]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
Diethyl azodicarboxylate (0.101 ml) was added dropwise to a stirred mixture of 4-(6-chlorobenzofuran-7-ylamino)-7-hydroxy-6-methoxyquinazoline (0.1 g), 1-(2-hydroxyethyl)pyrrolidine (0.04 g), triphenylphosphine (0.169 g) and methylene chloride (5 ml) and the reaction mixture was stirred at ambient temperature for 2 hours. The solvent was evaporated and the residue was purified by column chromatography on silica using increasingly polar mixture of methylene chloride and a saturated methanolic ammonia solution as eluent. There was thus obtained the title compound (0.033 g) as a solid; NMR Spectrum: (DMSOd6 and CF3CO2D) 1.9 (m, 2H), 2.1 (m, 2H), 3.2 (m, 2H), 3.65-3.85 (m, 4H), 4.05 (s, 3H), 4.6 (m, 2H), 7.15 (d, 1H), 7.45 (s, 1H), 7.6 (d, 1H), 7.8 (d, 1H), 8.1 (d, 1H), 8.25 (s, 1H), 8.85 (s, 1H); Mass Spectrum: M+H+ 439.
後処理
- customThe solvent was evaporated
- customthe residue was purified by column chromatography on silica using
- temperatureincreasingly polar
- additionmixture of methylene chloride
出典と根拠
- ORDレコード
- ord-5775e14afd58470c9edbd4621bc817c6
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06849625B2
関連ノート
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