HRID12821

反应详情

EQUATION

反应方程式

HRID 12821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-Cyclopropyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (140 mg, 0.56 mmol) in CH3OH (2 mL) and water (2 mL) was added LiOH (16 mg, 0.67 mmol). The reaction mixture was stirred at reflux overnight, and then the solution was concentrated under reduced pressure to remove the methanol. The residue was diluted with water and the solution was acidified to pH 2 with concentrated HCl. The resulting mixture was then extracted with ethyl acetate three times. The combined organic extracts were concentrated in vacuo to give 1-cyclopropyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (130 mg, quantitative), which was used without further purification.

WORKUP

后处理

  1. temperatureat reflux overnight
  2. concentrationthe solution was concentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionThe resulting mixture was then extracted with ethyl acetate three times
  6. concentrationThe combined organic extracts were concentrated in vacuo