反応式
Br[CH2:2][CH2:3][C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[NH:10][C:9](=[O:17])[C:8]2[N:18]([CH3:22])[CH:19]=[C:20]([CH3:21])[C:7]1=2)=[O:5].[CH3:23][N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1>O1CCOCC1>[CH3:22][N:18]1[C:8]2[C:9](=[O:17])[NH:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:6]([C:4](=[O:5])[CH2:3][CH2:2][N:27]3[CH2:28][CH2:29][N:24]([CH3:23])[CH2:25][CH2:26]3)[C:7]=2[C:20]([CH3:21])=[CH:19]1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
1.5 g of 4-(3-bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one and 0.85 g of N-methylpiperazine are warmed at 80° C. for 15 hours in 50 ml of dioxane. The thus-obtained mixture is concentrated to dryness in vacuo. 20 ml of saturated aqueous sodium carbonate solution are added thereto with stirring, and the mixture is then extracted three times with ethyl acetate. The combined extracts are dried over sodium sulfate, and the solvent is stripped off in vacuo. The resulting residue is chromatographed on neutral silica gel (methylene chloride/methanol 95/05). 1.2 g of the title compound of m.p. 187° C. (from isopropanol) are obtained).
後処理
- concentrationThe thus-obtained mixture is concentrated to dryness in vacuo
- addition20 ml of saturated aqueous sodium carbonate solution are added
- extractionthe mixture is then extracted three times with ethyl acetate
- dry with materialThe combined extracts are dried over sodium sulfate
- customThe resulting residue is chromatographed on neutral silica gel (methylene chloride/methanol 95/05)
出典と根拠
- ORDレコード
- ord-5438a24a039444bb838c30312aec8c6f
- 出典データセット
- uspto-grants-1982_12
- 特許番号
- US04363816
関連ノート
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