HRID12828

反应详情

EQUATION

反应方程式

HRID 12828 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-tert-butyl-5-chloro-1H-pyrazole-4-carboxylic acid ethyl ester (5 g, 21.7 mmol) in methanol (50 mL) and water (50 mL) was added LiOH (0.63 g, 26.3 mmol). The reaction mixture was stirred at reflux overnight and then concentrated under reduced pressure to remove the methanol. The residue was diluted with water, acidified to pH 2 with concentrated HCl (4 mL), and extracted with ethyl acetate. The organic extracts were evaporated in vacuo to give 1-tert-butyl-5-chloro-1H-pyrazole-4-carboxylic acid (4 g, 91%) which was used without further purification.

WORKUP

后处理

  1. temperatureat reflux overnight
  2. concentrationconcentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. customThe organic extracts were evaporated in vacuo