HRID1292395

反应详情

EQUATION

反应方程式

HRID 1292395 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 3,5-dimethylphenylethyne (156 mg in 7 mL of dry, nitrogen saturated triethylamine) was added 2-iodo-4-nitroaniline (264 mg, prepared essentially as described in: Toth, I. Helv. Chim. Acta, 1971, 54, 1486.) followed by tetrakis(triphenylphosphine)palladium (23 mg) and cuprous bromide (10 mg) and the mixture heated to reflux on an oil bath. After 2 hours the mixture was cooled to room temperature, concentrated in vacuo and purified by flash chromatography on silica gel (hexane:methylene chloride:ethyl acetate, 15:8:1) to give the title compound (256 mg).

WORKUP

后处理

  1. customprepared essentially
  2. temperaturethe mixture heated
  3. temperatureto reflux on an oil bath
  4. concentrationconcentrated in vacuo
  5. custompurified by flash chromatography on silica gel (hexane:methylene chloride:ethyl acetate, 15:8:1)