HRID1005279

反应详情

EQUATION

反应方程式

HRID 1005279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 10 g (26 mmol) of 3-(4-chloro-3-nitrophenyl)-1-methyl-4,5-di(trifluoromethyl)-1H-pyrazole in 50 ml of methanol was added dropwise to a mixture, heated at reflux temperature, of 4.5 g (80 mmol) of iron powder and 30 ml of glacial acetic acid. After the mixture had been stirred for 3 hours it was poured into 100 ml of water. Then, 100 ml of ethyl acetate were added to the mixture. The solids were subsequently separated off from the mixture and washed with ethyl acetate. The organic phase was separated off from the combined filtrates, washed with water, dried over magnesium sulfate and finally concentrated.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux temperature
  3. customThe solids were subsequently separated off from the mixture
  4. washwashed with ethyl acetate
  5. customThe organic phase was separated off from the combined filtrates
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationfinally concentrated