反応式
[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[C:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=2)=[N:11][C@@H:10]([NH:25][C:26]([NH:28][C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([N:35]([CH3:37])[CH3:36])[CH:30]=2)=[O:27])[C:9]1=[O:38])=[O:6])([CH3:4])([CH3:3])[CH3:2].C(O)C.[ClH:42]>C(O)C>[ClH:42].[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[C:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=2)=[N:11][C@@H:10]([NH:25][C:26]([NH:28][C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([N:35]([CH3:37])[CH3:36])[CH:30]=2)=[O:27])[C:9]1=[O:38])=[O:6])([CH3:4])([CH3:2])[CH3:3]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 50 °C
実験手順
N-((3R)-1-tert-Butylcarbonylmethyl-2,3-dihydro-2-oxo-5-(2-pyridyl)-1H-1,4-benzodiazepin-3-yl)-N'-(3-dimethylaminophenyl)urea (70 g, 136.6 mmol) was taken up in ethanol (1 l) and 2.26M HCl ethanol (63.5 ml, 143.4 mmol) was added dropwise. The mixture was warmed up to 50° C. to afford a clear solution, which was seeded, cooled to 0° C. and stirred at the same temperature overnight. The resultant precipitate was collected by flirtation to provide the title compound as a white crystalline (62.4 g, 82%): top. 181°-184° C.
後処理
- customto afford a clear solution, which
- temperaturecooled to 0° C.
- customThe resultant precipitate was collected by flirtation
出典と根拠
- ORDレコード
- ord-55f511a55d61454a83be8c226edee531
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728829
関連ノート
読み込み中…