Reaktionsgleichung
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH:9]=O)=[CH:4][CH:3]=1.[NH2:12][CH2:13][C:14]([NH2:16])=[O:15].[OH-].[Na+].Cl.C(=O)(O)[O-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]=[CH:13][C:14]([OH:15])=[N:16][CH:9]=2)=[CH:6][CH:7]=1Komponenten
7
Edukt 5
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- -30 °C
Versuchsvorschrift
To a stirred solution of (4-chloro-phenyl)-oxo-acetaldehyde (300 mg, 1.69 mmol) in methanol (15 mL) was added 2-amino-acetamide (187 mg, 1.69 mmol). The resulting mixture was cooled to −30° C. and 12.5M aqueous sodium hydroxide solution (0.3 mL) added. The resulting mixture was allowed to warm to −5° C. and was stirred at this temperature for 2 hours, followed by stirring at room temperature for 2 hours. Concentrated aqueous hydrogen chloride (0.3 mL) was added, followed by saturated sodium bicarbonate solution (1.0 mL). The reaction mixture was filtered and the resulting solid was washed with water (10 mL) and dried in a vacuum oven to afford the title compound as a brown solid (130 mg, 37%)
Aufarbeitung
- temperatureto warm to −5° C.
- stirringby stirring at room temperature for 2 hours
- filtrationThe reaction mixture was filtered
- washthe resulting solid was washed with water (10 mL)
- customdried in a vacuum oven
Quellen und Nachweise
- ORD-Eintrag
- ord-bacc7dfb8db14fada60bd2545ce4e55c
- Quelldatensatz
- uspto-grants-2012_10
- Patentnummer
- US08278343B2
Verknüpfte Notizen
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