HRID1766352

反应详情

EQUATION

反应方程式

HRID 1766352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Formyl-1-benzofuran-5-carbonitrile (157 mg, 0.915 mmol) and ethyl cyanoacetate (103 mg, 0.915 mmol) are dissolved in ethanol (8 ml). Piperidine (2.3 mg, 0.027 mmol) is added, and the reaction mixture is stirred for two hours at room temperature. A solution of Example 1A (253 mg, 0.915 mmol) and piperidine (7.8 mg, 0.091 ml) in ethanol (2 ml) is added, and the reaction mixture is stirred at reflux (95° C.) overnight (18 h). The crude reaction mixture is concentrated in vacuo, dissolved in DMSO (7 ml) and purified by preparative HPLC.

WORKUP

后处理

  1. stirringthe reaction mixture is stirred
  2. temperatureat reflux (95° C.) overnight (18 h)
  3. customThe crude reaction mixture
  4. concentrationis concentrated in vacuo
  5. dissolutiondissolved in DMSO (7 ml)
  6. custompurified by preparative HPLC