Dimethylformamide → 5-phenylvalerylamino-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one
Reaktionsgleichung
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(Cl)(Cl)=O.ClCCl.N[C:22]1[CH:38]=[CH:37][C:36]2[C:27]3[NH:28][C:29](=[O:35])[C:30]4[N:31]([CH:32]=[CH:33][N:34]=4)[C:26]=3[CH2:25][C:24]=2[CH:23]=1.C[N:40](C)C=O>>[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][C:11]([NH:40][C:32]2[N:31]3[C:26]4[CH2:25][C:24]5[CH:23]=[CH:22][CH:38]=[CH:37][C:36]=5[C:27]=4[NH:28][C:29](=[O:35])[C:30]3=[N:34][CH:33]=2)=[O:13])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1Komponenten
6
Versuchsvorschrift
The preparation is carried out as in Example 12, from 5 g of 5-phenylvaleric acid, 2.5 ml of thionyl chloride, 60 ml of dichloromethane, 1 g of 8-amino-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one and 75 ml of dimethylformamide. After refluxing for 7 hours, the insoluble material is filtered and recrystallized from dimethylformamide. After filtration, washing with water and drying under reduced pressure (1 mm Hg, 0.13 kPa) at 80° C., there is obtained 0.58 g of 8-(5-phenylvalerylamino-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one in the form of a yellow solid which decomposes at 170° C. (Analysis C24H22N4O2.0.41DMF, % calculated C: 72.34, H: 5.56, N: 14.06, % found C: 72.0, H: 5.6, N: 13.8).
Aufarbeitung
- temperatureAfter refluxing for 7 hours
- filtrationthe insoluble material is filtered
- customrecrystallized from dimethylformamide
- filtrationAfter filtration
- washwashing with water
- customdrying under reduced pressure (1 mm Hg, 0.13 kPa) at 80° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-3d88c839167a4ddaaf5796f47fd5cd1a
- Quelldatensatz
- uspto-grants-1998_08
- Patentnummer
- US05789406
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