反応式
Cl.CN(C)CCCN=C=NCC.OC1C=CC=C[N+]=1[O-].[CH3:21][O:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][C:32]=1[O:33][CH3:34])[N:29]=[CH:28][N:27]=[C:26]2[O:35][C:36]1[CH:41]=[CH:40][C:39]([CH2:42][C:43]([OH:45])=O)=[CH:38][CH:37]=1.[NH2:46][C:47]1[CH:52]=[CH:51][C:50]([N:53]([CH3:55])[CH3:54])=[CH:49][N:48]=1.C(N(C(C)C)CC)(C)C.CO[C@@H]1[C@@H](C(OC)=O)[C@@H]2[C@@H](CN3[C@H](C2)C2NC4C=C(OC)C=CC=4C=2CC3)C[C@H]1OC(C1C=C(OC)C(OC)=C(OC)C=1)=O>CN(C=O)C>[CH3:54][N:53]([CH3:55])[C:50]1[CH:51]=[CH:52][C:47]([NH:46][C:43](=[O:45])[CH2:42][C:39]2[CH:38]=[CH:37][C:36]([O:35][C:26]3[C:25]4[C:30](=[CH:31][C:32]([O:33][CH3:34])=[C:23]([O:22][CH3:21])[CH:24]=4)[N:29]=[CH:28][N:27]=3)=[CH:41][CH:40]=2)=[N:48][CH:49]=1参加物
反応物 6
生成物 1
試薬・触媒・溶媒 1
実験手順
1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.101 g) and 2-hydroxypyridine N-oxide (0.059 g) were added in turn to a stirred mixture of 2-[4-(6,7-dimethoxyquinazolin-4-yloxy)phenyl]acetic acid (0.15 g), 2-amino-5-dimethylaminopyridine (0.073 g), diisopropylethylamine (0.092 ml) and DMF (2 ml) and the resultant mixture was stirred at ambient temperature for 16 hours. The resultant reaction mixture was transferred onto a Waters ‘β Basic Hypersil’ reversed-phase preparative HPLC column (5 microns silica, 30 mm diameter, 250 mm length) that was eluted with decreasingly polar mixtures of water (containing 0.2% ammonium carbonate) and acetonitrile as eluent. There was thus obtained the title compound (0.148 g); 1H NMR: (DMSOd6) 2.88 (s, 6H), 3.71 (s, 2H), 3.98 (s, 3H), 3.98 (s, 3H), 7.19 (m, 1H), 7.25 (d, 2H), 7.38 (s, 1H), 7.44 (d, 2H), 7.55 (s, 1H), 7.84 (d, 1H), 7.90 (d, 1H), 8.53 (s, 1H), 10.43 (s, 1H); Mass Spectrum: M+H+ 460.
後処理
- customThe resultant reaction mixture
- washwas eluted with decreasingly polar mixtures of water (containing 0.2% ammonium carbonate) and acetonitrile as eluent
出典と根拠
- ORDレコード
- ord-d3d4abec0e974059a69ce6da66cdfd06
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08153643B2
関連ノート
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