Reaktionsgleichung
[F:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[C:5]([N+:12]([O-])=O)=[N:4][CH:3]=1.[H][H]>C(O)(=O)C.C(=O)([O-])[O-].[Ca+2].[Pd+2].C(=O)([O-])[O-]>[NH2:12][C:5]1[C:6]([C:8]([O:10][CH3:11])=[O:9])=[N:7][C:2]([F:1])=[CH:3][N:4]=1Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
In 1.0 mL of acetic acid was dissolved 20 mg of methyl 6-fluoro-3-nitro-2-pyrazinecarboxylate. After adding 6 mg of lead-poisoned palladium-calcium carbonate, hydrogen gas was introduced into the mixture at room temperature under a pressure of 1 atmosphere, until the mixture became absorbing no further quantity of hydrogen gas. The insoluble matter was filtered off from the reaction mixture, and the filtrate was concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1] to obtain 2 mg of methyl 3-amino-6-fluoro-2-pyrazinecarboxylate as a light yellow-colored solid product.
Aufarbeitung
- additionwas introduced into the mixture at room temperature under a pressure of 1 atmosphere, until the mixture
- custombecame absorbing no further quantity of hydrogen gas
- filtrationThe insoluble matter was filtered off from the reaction mixture
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue thus obtained
- customwas purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1]
Quellen und Nachweise
- ORD-Eintrag
- ord-27d2ce7a66aa4c38ae6390899a0cf153
- Quelldatensatz
- uspto-grants-2004_10
- Patentnummer
- US06800629B2
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