HRID2195688

反应详情

EQUATION

反应方程式

HRID 2195688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4 g of malonitrile is dissolved in 50 ml of dimethylformamide. To the solution, in several portions, 2.4 g of 60% sodium hydride in oily dispersion are added. To the clear solution 8 g of 5-(2,6-dimethylmorpholin-4-yl)isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The reaction mixture is diluted with 70 ml of water and extracted with 2×30 ml of ethyl acetate. The aqueous phase is evaporated in vacuum, the solid residue is dissolved in 20 ml of water, and the pH is set to 6. The precipitated material is filtered off, washed with water. After drying 6.5 g of the title compound is obtained. (MH+: 299)

WORKUP

后处理

  1. extractionextracted with 2×30 ml of ethyl acetate
  2. customThe aqueous phase is evaporated in vacuum
  3. dissolutionthe solid residue is dissolved in 20 ml of water
  4. filtrationThe precipitated material is filtered off
  5. washwashed with water
  6. dry with materialAfter drying 6.5 g of the title compound
  7. customis obtained