HRID1470660

反应详情

EQUATION

反应方程式

HRID 1470660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customcompletion of the reaction
  2. concentrationThe reaction mixture was concentrated
  3. temperaturethe resulting residue was cooled
  4. extractionextracted with ethyl acetate
  5. washThe combined organic layers were washed with water, brine
  6. dry with materialdried over anhydrous sodium sulphate
  7. concentrationthen concentrated
  8. customThe resulting residue was purified
  9. washby washing with hot hexane