HRID470610

反应详情

EQUATION

反应方程式

HRID 470610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

4-methoxy-3-nitro-benzaldehyde (compound of Example 5; 1.05 g, 5.79 mmol) and malonic acid (1.32 g, 1.27 mmol) were dissolved in pyridine (20 mL) under stirring and piperidine (1 mL) was added to the pyridine solution. The reaction mixture was heated at 75° C. to 80° C. for 3 h, after which the temperature was further increased to 120° C. and maintained at this temperature for 6 h. At the end of the reaction, pyridine was evaporated, followed by addition of aqueous HCl (1:1) to obtain pH ˜4. The solid obtained was filtered, washed with cold water and dried.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated at 75° C. to 80° C. for 3 h
  2. temperaturemaintained at this temperature for 6 h
  3. customwas evaporated
  4. additionfollowed by addition of aqueous HCl (1:1)
  5. customto obtain pH ˜4
  6. customThe solid obtained
  7. filtrationwas filtered
  8. washwashed with cold water
  9. customdried