HRID232016

反应详情

EQUATION

反应方程式

HRID 232016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Oxalyl chloride (2.8 g; 0.022 mol) is added to a suspension of compound 3 (4.1 g; 0.022 mol) in dichloromethane (50 cc). The mixture is heated under reflux until gas evolution ceases and then treated with a solution of trichloroethanol (3.3 g; 0.022 mol) and pyridine (3.5 g; 0.044 mol) in dichloromethane (30 cc). The mixture is then treated with water and then dried. After evaporation of the solvent and crystallization in pentane, 2,2,2-tri-chloroethyl 2-cyanonicotinate (4.55 g; m.p. 103° C.) is obtained (yield=78%).

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux until gas evolution ceases
  3. customdried
  4. customAfter evaporation of the solvent and crystallization in pentane