HRID639158

反应详情

EQUATION

反应方程式

HRID 639158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under argon, 100 mg (0.44 mmol) of the compound of Example 2A, 57.97 mg (0.44 mmol) 4-formylbenzonitrile and 37.17 mg (0.44 mmol) 2-cyanoacetamide are dissolved in 2 ml ethanol. 3.76 mg (4.4 μl, 0.04 mmol) piperidine are added and the mixture is stirred at reflux overnight. The product is crystallised from the reaction mixture at 4° C. The formed crystals are filtered, washed twice with ethanol and dried. The crude product is purified by column chromatography with dichloromethane/methanol 100:1 as eluent.

WORKUP

后处理

  1. temperatureat reflux overnight
  2. customThe product is crystallised from the reaction mixture at 4° C
  3. filtrationThe formed crystals are filtered
  4. washwashed twice with ethanol
  5. customdried
  6. customThe crude product is purified by column chromatography with dichloromethane/methanol 100:1 as eluent