HRID1187356

反应详情

EQUATION

反应方程式

HRID 1187356 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,6-dichloronicotinic acid (5.005 g, 26.18 mmol) in DCM (60 ML) was added a few drops of DMF followed by the addition dropwise of oxalyl chloride (2.27 mL, 26.18 mmol). The reaction was stirred at room temperature for two hours until gas bubbling had stopped. The solvent was evaporated under reduced pressure to give an oil. DCM (60 mL) was added and the reaction mixture was cooled in an ice bath. Cyclohexylamine (5.98 mL, 52.36 mmol) was added slowly keeping the temperature below 15° C. The reaction was stirred at room temperature overnight.

WORKUP

后处理

  1. custombubbling
  2. customThe solvent was evaporated under reduced pressure
  3. customto give an oil
  4. temperaturethe reaction mixture was cooled in an ice bath
  5. customthe temperature below 15° C
  6. stirringThe reaction was stirred at room temperature overnight