HRID1428717

反应详情

EQUATION

反应方程式

HRID 1428717 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The ethyl 2-(3-fluoro-4-(methylsulfonamidomethyl)phenyl)propanoate (12.5 g, 40.4 mmol) was dissolved in tetrahydrofuran-water mixture (120 mL, 2:1), lithium hydroxide (2.8 g, 121.1 mmol) was added and refluxing carried out for 12 h. After evaporation of the organic solvent under reduced pressure, the reaction mixture was extracted with diethyl ether (2×100 mL). The aqueous layer was acidified using 1 N HCl solution to pH=2 and extracted with dichloromethane (3×250 mL). The combined organic layer was dried over magnesium sulfate and concentrated under reduced pressure to afford 2-(3-fluoro-4-(methylsulfonamido-methyl)phenyl)propanoic acid (9.56 g, 86%).

WORKUP

后处理

  1. temperaturerefluxing
  2. customAfter evaporation of the organic solvent under reduced pressure
  3. extractionthe reaction mixture was extracted with diethyl ether (2×100 mL)
  4. extractionextracted with dichloromethane (3×250 mL)
  5. dry with materialThe combined organic layer was dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure