Reaktionsgleichung
[C:1]([CH:3]([N:11]=C(C1C=CC=CC=1)C1C=CC=CC=1)[C:4]([NH:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5])#[N:2].C(OCC)(=O)C.[ClH:31]>C(Cl)Cl>[ClH:31].[NH2:11][CH:3]([C:1]#[N:2])[C:4]([NH:6][C:7]([CH3:8])([CH3:10])[CH3:9])=[O:5]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
2-Cyano-N-(1,1-dimethylethyl)-2-[(diphenylmethylene)amino]acetamide 4 (900 g. 2.818 mol), ethyl acetate (4.5 L) and aqueous HCl (1 N. 4.5 L) were placed into a 12 L three-necked flask equipped with a nitrogen inlet, a gas outlet tube, reflux condenser, thermometer, mechanical stirrer, and maintained under a positive pressure of nitrogen. The mixture was heated on an oil bath at 60° C. for 4 hours with vigorous stirring, gradually cooled to room temperature, and then slowly diluted with CH2Cl2 (4 L). (Thin layer chromatography (EtOAc/hexanes=1/4) indicated no more starting material was present.) The resulting layers were separated and the aqueous phase was extracted with CH2Cl2 (4 L). The combined organic solutions were extracted with aqueous HCl (1 N, 2×0.5 L). The aqueous extracts were combined and concentrated under reduced pressure to yield 490 g (2.557 mol) of 2-amino-2-cyano-N-(1,1-dimethylethyl)-acetamide hydrochloride 5.HCl.
Aufarbeitung
- customequipped with a nitrogen inlet, a gas outlet tube
- temperaturereflux condenser
- temperaturethermometer, mechanical stirrer, and maintained under a positive pressure of nitrogen
- temperaturegradually cooled to room temperature
- custom) The resulting layers were separated
- extractionthe aqueous phase was extracted with CH2Cl2 (4 L)
- extractionThe combined organic solutions were extracted with aqueous HCl (1 N, 2×0.5 L)
- concentrationconcentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-430da2d36fa44eec9014d4707e973baa
- Quelldatensatz
- uspto-grants-2006_08
- Patentnummer
- US07087751B2
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