반응 #42857

반응 방정식

2,2-dimethylglutaric acid

urea

→

3,3-dimethylpiperidin-2,6-dione

수율 86.2%

용매

water

반응 조건

후처리

1. 1
   온도the mixture was cooled to near room temperature
2. 2
   추출The mixture was extracted with ethyl acetate three times
3. 3
   세척The organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated

실험 절차

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.

출처