HRID889063

反应详情

EQUATION

反应方程式

HRID 889063 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

To a stirred solution of 1-[5-Oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidin-3-ylmethyl]-1H-pyrazole-4-carboxylic acid ethyl ester (2.6 g, 6.81 mmol) in 14 mL MeOH:H2O (3:11), NaOH (0.4 g, 10.5 mmol) was added at room temperature. The mixture was heated at 100° C. for 2 h. The reaction mixture was cooled; MeOH was removed under reduced pressure, diluted with water, washed with DCM and acidified with 1% HCl. The acidified mixture was extracted with EtOAc (3×50 mL) and the combined extract was washed with brine, dried with Na2SO4, evaporated under reduced pressure to give the title compound in 88% yield (2.1 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customMeOH was removed under reduced pressure
  3. additiondiluted with water
  4. washwashed with DCM
  5. extractionThe acidified mixture was extracted with EtOAc (3×50 mL)
  6. extractionthe combined extract
  7. washwas washed with brine
  8. dry with materialdried with Na2SO4
  9. customevaporated under reduced pressure