HRID1020876

反应详情

EQUATION

反应方程式

HRID 1020876 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

4-Hydroxy-2-trifluoromethylpyridine (6.4 g, 39 mmol) was dissolved in 1,2-dichlorobenzene (64 g). Thionylchloride (23.2 g, 195 mmol) and DMF (10 drops) were added to the reaction mixture which was then heated to 70 to 80° C. After about 2 hours the reaction was completed and excess thionyl chloride was removed at an elevated temperature. The desired product was distilled under reduced pressure (50° C., 15 mbar) to yield 4-chloro-2-trifluoromethyl-pyridine (6.5 g, 36 mmol, yield: 92%). If required, remaining DMF was removed using an aqueous work-up.

WORKUP

后处理

  1. customexcess thionyl chloride was removed at an elevated temperature
  2. distillationThe desired product was distilled under reduced pressure (50° C., 15 mbar)