HRID536036

反应详情

EQUATION

反应方程式

HRID 536036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
52.5 °C

PROCEDURE

实验过程

1-[1-(2,4-Difluoro-phenyl)-5-oxo-pyrrolidin-3-ylmethyl]-1H-pyrazole-4-carboxylic acid ethyl ester (0.222 g, 0.62 mmol) was dissolved in a mixture of solvents Methanol:water (3:1, 5 ml) and KOH (0.07 g, 125 mmol) was added to the reaction mixture and then stirred at 50-55° C. for 3 hours. Solvents were removed and the residue was diluted with water (3 ml) and washed with DCM (3×10 ml) and acidified with dil. HCl. It was extracted with ethyl acetate (3×15 ml), organic layers were mixed and washed with brine (20 ml), dried over Na2SO4 and evaporated to dryness to obtain 1-[1-(2,4-Difluoro-phenyl)-5-oxo-pyrrolidin-3-ylmethyl]-1H-pyrazole-4-carboxylic acid (0.18 g, 90%) as a brownish sticky mass.

WORKUP

后处理

  1. additionwas added to the reaction mixture
  2. customSolvents were removed
  3. additionthe residue was diluted with water (3 ml)
  4. washwashed with DCM (3×10 ml)
  5. extractionIt was extracted with ethyl acetate (3×15 ml), organic layers
  6. additionwere mixed
  7. washwashed with brine (20 ml)
  8. dry with materialdried over Na2SO4
  9. customevaporated to dryness