反应 #42857

ord-839758e16358461ea01e3ad93e9d6318

溶剂

反应条件

温度
160°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07732448B2uspto-grants-2010_06