HRID1875438

反应详情

EQUATION

反应方程式

HRID 1875438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Under argon, 200 mg (0.86 mmol) of 2-iodophenylhydrazine, 133 mg (1.11 mmol) of 2-fluoro-phenylacetylene, 30 mg (0.04 mmol) of bis(triphenylphosphine)palladium(II) chloride and 8 mg (0.04 mmol) of copper(I) iodide are introduced into a mixture of 1.5 ml of triethylamine and 3.5 ml of benzene. The mixture is heated to reflux for 4 h and then diluted with ethyl acetate and filtered. The filtrate is concentrated and the residue is purified by preparative HPLC. 36 mg (18% of theory) of the desired product are obtained.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 4 h
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated
  5. customthe residue is purified by preparative HPLC