HRID406574

反应详情

EQUATION

反应方程式

HRID 406574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-4-nitro-1H-pyrazole (i.e. the product of Step A) (0.2 g, 0.74 mmol), iron powder (0.2 g, 3.6 mmol) and saturated aqueous ammonium chloride solution (1 mL) in ethanol (5 mL) was heated at 80° C. for 4 h. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and filtered through a pad of Celite® (diatomaceous earth) on a sintered glass frit funnel. The filtrate was concentrated under reduced pressure and the resulting material was purified by silica gel column chromatography (ethyl acetate as eluant) to provide the title compound (0.14 g).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationfiltered through a pad of Celite® (diatomaceous earth) on a sintered glass frit funnel
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe resulting material was purified by silica gel column chromatography (ethyl acetate as eluant)