HRID268965

反应详情

EQUATION

反应方程式

HRID 268965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

A mixture of 5-bromo-3-trifluoromethyl-pyridin-2-ylamine (example C.18 step 3) (723 mg, 3 mmol), sodium iodide (900 mg, 6 mmol), copper (I) iodide (29 mg, 5 mol %) and N,N′-dimethylethylendiamine (26 mg, 10 mol %) in n-butanol (6 mL) was stirred at reflux under argon atmosphere for 18 h. The reaction mixture was cooled to 23° C., extracted with ethyl acetate and water, the organic layers were dried over MgSO4, filtered and evaporated to leave the title compound as a brown solid (880 mg, 102%), which was used without further purification. MS (ISN) 287.0 [(M−H)−].

WORKUP

后处理

  1. temperatureat reflux under argon atmosphere for 18 h
  2. extractionextracted with ethyl acetate and water
  3. dry with materialthe organic layers were dried over MgSO4
  4. filtrationfiltered
  5. customevaporated