Sodium Carbonate → trans-3,7-dimethylhexahydro-1H-azepine-2-one
Reaktionsgleichung
[CH3:1][C@H:2]1[CH2:7][CH2:6][CH2:5][C@H:4]([CH3:8])[C:3]1=[N:9]O.C(=O)([O-])[O-:12].[Na+].[Na+]>C1(C)C(C)=CC=CC=1>[CH3:1][C@H:2]1[CH2:7][CH2:6][CH2:5][C@H:4]([CH3:8])[NH:9][C:3]1=[O:12]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
Into 20 ml of xylene were added 1.3 g of trans-2,6-dimethylcyclohexanone oxime and 6 g of polyphosphoric acid, the mixture was stirred for 10 hours at 100° C. The reaction mixture was cooled to near room temperature, poured into ice-water. Sodium carbonate was added to the mixture, and the mixture was extracted with ethyl acetete three times. The organic layers was 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 1.2 g of trans-3,7-dimethylhexahydro-1H-azepine-2-one.
Aufarbeitung
- temperatureThe reaction mixture was cooled to near room temperature
- extractionthe mixture was extracted with ethyl acetete three times
- washThe organic layers was washed with a saturated sodium chloride aqueous solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-02eb9cc3a411451bbbc32fea832d13af
- Quelldatensatz
- uspto-grants-2012_03
- Patentnummer
- US08129526B2
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