HRID626282

反应详情

EQUATION

反应方程式

HRID 626282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Phenyl-3-difluoromethyl-5-trifluoromethyl-4-pyrazolecarboxylic acid ethyl ester (3.0 g, 9.0 mmol) in ethanol (15 ml) was admixed gradually with an 8N aqueous sodium hydroxide solution (3.4 ml) and stirred at room temperature for 3 h. The solvent was removed by rotary evaporation; the residue was taken up in water (40 ml) and extracted with diethyl ether (20 ml). Acidification to pH 1 with 6M HCl was followed by extraction with ethyl acetate (3×30 ml). The combined organic phases were dried over sodium sulphate and filtered, and the solvent was removed by rotary evaporation. N-Phenyl-3-difluoromethyl-5-trifluoromethyl-4-pyrazolecarboxylic acid (2.58 g, 8.43 mmol, 94%) was isolated as a colourless solid.

WORKUP

后处理

  1. customThe solvent was removed by rotary evaporation
  2. extractionextracted with diethyl ether (20 ml)
  3. extractionAcidification to pH 1 with 6M HCl was followed by extraction with ethyl acetate (3×30 ml)
  4. dry with materialThe combined organic phases were dried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent was removed by rotary evaporation