Reaktionsgleichung
[CH2:1]([O:3][C:4](=[O:16])[C:5](=O)[CH2:6][C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:8])[CH3:2].[NH:17]([C:19]1[CH:20]=[CH:21][C:22]([O:25][CH3:26])=[N:23][CH:24]=1)[NH2:18]>C(O)C>[CH2:1]([O:3][C:4]([C:5]1[CH2:6][C:7]([OH:8])([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:17]([C:19]2[CH:24]=[N:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)[N:18]=1)=[O:16])[CH3:2]Komponenten
4
Versuchsvorschrift
4-(2-Pyridyl)-2,4-dioxobutanoic acid ethyl ester (1.10 g) obtained from Referential Example 31 and 5-hydrazino-2-methoxypyridine (0.692 g) obtained from Referential Example 2 were dissolved in ethanol (22 mL). The resultant mixture was refluxed under heat for 14 hours, followed by cooling in air. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate), followed by purification through silica gel column chromatography (toluene-acetone), to thereby give 5-hydroxy-1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)-4,5-dihydropyrazole-3-carboxylic acid ethyl ester as a solid substance (0.575 g, 34%).
Aufarbeitung
- temperatureunder heat for 14 hours
- temperatureby cooling in air
- customThe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate)
- customfollowed by purification through silica gel column chromatography (toluene-acetone)
Quellen und Nachweise
- ORD-Eintrag
- ord-170b13e042244dee9a638a215342bbcf
- Quelldatensatz
- uspto-grants-2009_11
- Patentnummer
- US07622471B2
Verknüpfte Notizen
Wird geladen…