HRID1470660
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To the solution of 4-(2,5-dimethyl-pyrrol-1-yl)-2,3,5,6-tetrafluoro-benzoic acid methyl ester (0.6 g, 1.99 mmol) in THF (20 mL) was added an aq. solution of 5 N NaOH (5 mL). The reaction mixture was stirred under refluxed at 90° C. for 3 hours. TLC shows completion of the reaction. The reaction mixture was concentrated and the resulting residue was cooled, acidified with aq, solution of 2 N HCl, extracted with ethyl acetate. The combined organic layers were washed with water, brine and dried over anhydrous sodium sulphate then concentrated. The resulting residue was purified by washing with hot hexane to get the title compound (0.43 g, 75%). LCMS− m/z 288, 91%
WORKUP
后处理
- customcompletion of the reaction
- concentrationThe reaction mixture was concentrated
- temperaturethe resulting residue was cooled
- extractionextracted with ethyl acetate
- washThe combined organic layers were washed with water, brine
- dry with materialdried over anhydrous sodium sulphate
- concentrationthen concentrated
- customThe resulting residue was purified
- washby washing with hot hexane