Reaktionsgleichung
[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8](O)=[O:9])[C:3](O)=[O:4].[NH2:12]C(N)=O>O>[CH3:1][C:2]1([CH3:11])[CH2:6][CH2:7][C:8](=[O:9])[NH:12][C:3]1=[O:4]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 160 °C
Versuchsvorschrift
The mixture of 10 g of 2,2-dimethylglutaric acid and 37.5 g of urea was stirred for 8 hours at 160° C. Into the reaction mixture was added water at 100° C., and the mixture was cooled to near room temperature. The mixture was extracted with ethyl acetate three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 7.6 g of 3,3-dimethylpiperidin-2,6-dione.
Aufarbeitung
- temperaturethe mixture was cooled to near room temperature
- extractionThe mixture was extracted with ethyl acetate three times
- washThe organic layers were washed with a saturated sodium chloride aqueous solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-839758e16358461ea01e3ad93e9d6318
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07732448B2
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