反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[CH:21]=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.[CH3:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[CH2:31][C:32](Cl)=[O:33].C(N(CC)CC)C>ClCCl>[CH:23]1[CH:22]=[CH:21][N:13]2[CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[N:10]([C:8]([C:5]3[CH:4]=[CH:3][C:2]([NH:1][C:32](=[O:33])[CH2:31][C:26]4[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=4[CH3:24])=[N:7][CH:6]=3)=[O:9])[CH2:11][C:12]=12参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A mixture of 2.0 mmol of 10, 11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2.1 mmol of 2-methylbenzeneacetyl chloride and 5 mmol of triethylamine in 10 ml of dichloromethane is stirred under argon at room temperature for 16 hours. The solvent is removed under vacuum and the residue partitioned between 50 ml of ethyl acetate and 25 ml of water. The organic layer is separated, washed with H2O, 1N NaHCO3, brine and dried (Na2SO4). The solvent is removed and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.
後処理
- customThe solvent is removed under vacuum
- customthe residue partitioned between 50 ml of ethyl acetate and 25 ml of water
- customThe organic layer is separated
- washwashed with H2O, 1N NaHCO3, brine
- dry with materialdried (Na2SO4)
- customThe solvent is removed
- customthe residue chromatographed on silica gel with ethyl acetate-hexane as solvent
出典と根拠
- ORDレコード
- ord-fa9ad543ba63442b81d2d3bbf3850ef4
- 出典データセット
- uspto-grants-1996_07
- 特許番号
- US05536718
関連ノート
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