Reaktionsgleichung
[N:1]1[CH:6]=[CH:5][N:4]=[C:3](C(N)=O)[C:2]=1[C:10]([NH2:12])=[O:11].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Pb+4].C[N:31](C)[CH:32]=[O:33]>>[NH:31]1[C:3]2[N:4]=[CH:5][CH:6]=[N:1][C:2]=2[C:10](=[O:11])[NH:12][C:32]1=[O:33]Komponenten
4
Versuchsvorschrift
A 50 ml. flask was charged with 0.90 g. pyrazine-2,3-dicarboxamide dissolved in 16 ml. dimethylformamide. A 2.4 g. portion of lead tetra-acetate was added to the solution and the reaction mixture was stirred at 40° for 15 minutes. The reaction mixture was cooled, 30 g. of ice was added and after 1 hour the mixture was filtered. Crystallization of the residue from water gave, after drying in vacuo, a yield of 0.64 g. of pyrazino[2,3-d]pyrimidine-2,4(1H,3H)-dione, melting point 364°-365°, which represented 71 percent of theory. The structure was confirmed by infra-red spectroscopy.
Aufarbeitung
- additionflask was charged with 0.90 g
- temperatureThe reaction mixture was cooled
- additionof ice was added and after 1 hour the mixture
- filtrationwas filtered
- customCrystallization of the residue from water
- customgave
- customafter drying in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-9b9746177ea04820bf716dff36e758b5
- Quelldatensatz
- uspto-grants-1976_03
- Patentnummer
- US03947416
Verknüpfte Notizen
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