HRID232016
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture is heated
- temperatureunder reflux until gas evolution ceases
- customdried
- customAfter evaporation of the solvent and crystallization in pentane