反応式
[CH3:1][NH:2][CH2:3][CH2:4][C:5]([N:7]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:11](=[O:18])[NH:10][C:9]2[CH:19]=[CH:20][CH:21]=[CH:22][C:8]1=2)=[O:6].[CH3:23][C:24]1[CH:32]=[CH:31][C:27]([CH2:28][CH2:29]Br)=[CH:26][CH:25]=1.C(=O)([O-])O.[Na+]>C(#N)C>[CH3:23][C:24]1[CH:32]=[CH:31][C:27]([CH2:28][CH2:29][N:2]([CH2:3][CH2:4][C:5]([N:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11](=[O:18])[NH:10][C:9]3[CH:19]=[CH:20][CH:21]=[CH:22][C:8]2=3)=[O:6])[CH3:1])=[CH:26][CH:25]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A mixture of 5-(3-methylaminopropionyl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one (0.20 g) (J. Med. Chem., 1963, 6, 255), 4-methylphenethyl bromide (0.14 g) and sodium hydrogen carbonate (60 mg) in acetonitrile (20 ml) was heated under reflux for 16 hours and evaporated. The residue was partitioned between water and dichloromethane and the organic layer washed with brine, dried over MgSO4 and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-20% methanol as eluant. Appropriate fractions were combined and evaporated and the residue crystallised from ether to give the title compound as a colourless solid, 60 mg (21%).
後処理
- temperaturewas heated
- temperatureunder reflux for 16 hours
- customevaporated
- customThe residue was partitioned between water and dichloromethane
- washthe organic layer washed with brine
- dry with materialdried over MgSO4
- customevaporated
- customThe residue was purified by chromatography on silica
- customevaporated
- customthe residue crystallised from ether
出典と根拠
- ORDレコード
- ord-f317d4907b7246d2bd8a17afb1447994
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05418229
関連ノート
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