HRID254816

反应详情

EQUATION

反应方程式

HRID 254816 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 ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-3-carboxylate (3.0 g, 7.6 mmol) in acetic acid (30 ml) at room temperature was bubbled chlorine gas for 10 minutes. The reaction mixture was stirred at room temperature for 2 hours and the resulting solution was quenched with water (100 ml). The organic solution was extracted with diethyl ether (100 ml×2). With saturated sodium bicarbonate solution, remained acetic acid was removed and organic phase was evaporated with reduced pressure. The crude residue was purified with silica gel column (hexane/ethyl acetate=5/1) to produce title compound (3.1 g, 95% yield) as white solid.

WORKUP

后处理

  1. customthe resulting solution was quenched with water (100 ml)
  2. extractionThe organic solution was extracted with diethyl ether (100 ml×2)
  3. customwas removed
  4. customorganic phase was evaporated with reduced pressure
  5. customThe crude residue was purified with silica gel column (hexane/ethyl acetate=5/1)