Reaktion #42857

Reaktionsgleichung

2,2-dimethylglutaric acid

urea

→

3,3-dimethylpiperidin-2,6-dione

Ausbeute 86.2%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was cooled to near room temperature
2. 2
   ExtraktionThe mixture was extracted with ethyl acetate three times
3. 3
   WaschenThe organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   Einengenconcentrated

Vorschrift

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.

Quelle