HRID889063
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled
- customMeOH was removed under reduced pressure
- additiondiluted with water
- washwashed with DCM
- extractionThe acidified mixture was extracted with EtOAc (3×50 mL)
- extractionthe combined extract
- washwas washed with brine
- dry with materialdried with Na2SO4
- customevaporated under reduced pressure