HRID1816620

反应详情

EQUATION

反应方程式

HRID 1816620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2 ml ethyl 2,4-dioxovalerate and 1.2 g phenyl hydrazine were dissolved in 20 ml acetic acid, followed by stirring at 100° C. for 2 hours. After evaporating acetic acid, ethyl acetate was added to the residue. The mixture was washed with aqueous sodium hydrogencarbonate solution and brine, dried over anhydrous magnesium sulfate and evaporated. The residue was subjected to silica gel column chromatography, to give 0.37 g of ethyl 3-methyl-1-phenyl-1H-5-pyrazolecarboxylate with hexane:ethyl acetate (14:1) and 0.46 g of ethyl 5-methyl-1-phenyl-1H-3-pyrazolecarboxylate with hexane:ethyl acetate (9:1).

WORKUP

后处理

  1. customAfter evaporating acetic acid, ethyl acetate
  2. additionwas added to the residue
  3. washThe mixture was washed with aqueous sodium hydrogencarbonate solution and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated