反応 #42857

反応方程式

2,2-dimethylglutaric acid

urea

→

3,3-dimethylpiperidin-2,6-dione

収率 86.2%

溶媒

water

反応条件

後処理

1. 1
   温度the mixture was cooled to near room temperature
2. 2
   抽出The mixture was extracted with ethyl acetate three times
3. 3
   洗浄The organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated

実験手順

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.

出典