HRID1877407

反应详情

EQUATION

反应方程式

HRID 1877407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(2,5-dichloro-phenoxy)-5-fluoro-nicotinic acid (2.14 g, 7.08 mmol, 1.0 equiv; Example 80, Step 1) in dichloromethane (15 mL) was added thionyl chloride (16.4 g, 10 mL, 138 mmol, 19.5 equiv; [CAS RN 7719-09-7]) and the reaction mixture heated to reflux for 2 h. The reaction mixture was concentrated under reduced pressure and remaining thionyl chloride removed by azotropic distillation with toluene. The crude material was used in the consecutive reaction step without further purification.

WORKUP

后处理

  1. temperaturethe reaction mixture heated
  2. temperatureto reflux for 2 h
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customremoved by azotropic distillation with toluene
  5. customThe crude material was used in the consecutive reaction step without further purification