HRID714452

反应详情

EQUATION

反应方程式

HRID 714452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

5.5 g (24.64 mmol) of diethylpyridine 2,4-dicarboxylate (Example 50A) were dissolved in 55 ml of ethanol. 0.47 g (4.93 mmol) of magnesium chloride was added, and the mixture was then cooled to 0° C., 8.44 g (147.83 mmol) of cyclopropylamine were slowly added dropwise and the reaction mixture was stirred at 0° C. for 15 min and stirred further at RT for 2 days. The reaction mixture was evaporated. The residue was dissolved in water and extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulfate, filtered and concentrated using a rotary evaporator.

WORKUP

后处理

  1. stirringstirred further at RT for 2 days
  2. customThe reaction mixture was evaporated
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted three times with ethyl acetate
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customa rotary evaporator