Reaktionsgleichung
C=O.[Na].O=[C:5]([CH:11]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13])C(OCC)=O.C([O-])([O-])=O.[K+].[K+]>O>[C:12]([O:14][CH2:15][CH3:16])(=[O:13])[C:11]([C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)=[CH2:5]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
225 ml of 37 weight percent aqueous formaldehyde solution are added dropwise with stirring to a solution of 316 g of diethyl 2-oxo-3-phenylsuccinate sodium salt and 560 ml of water. During the addition, the mixture is maintained at a temperature below 25° C. The mixture is stirred for one hour at room temperature and then 152 g of anhydrous K2CO3 are added in portions over a ten minute period, while the temperature is maintained below 25° C. The resultant mixture is vigorously stirred for 1.5 hours at room temperature under a nitrogen atmosphere. The reaction mixture is diluted with 1500 ml of water and extracted with one 2.5 l. portion of ether followed by two 1.25 l portions of ether. The ether is removed and a product comprising an oil of ethyl atropate is obtained.
Aufarbeitung
- additionDuring the addition
- temperaturethe mixture is maintained at a temperature below 25° C
- temperatureis maintained below 25° C
- extractionextracted with one 2.5 l
- customThe ether is removed
- customis obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-8aaf974f22b14fd5b5561505aebcd1ba
- Quelldatensatz
- uspto-grants-1983_05
- Patentnummer
- US04382141
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