HRID553602

反应详情

EQUATION

反应方程式

HRID 553602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.64 g (6.31 mmol) of 2-(2,3-difluoro-phenylsulfanyl)-2-methyl-propionic acid ethyl ester in THF (165 mL) at room temperature are added 1.62 g (12.6 mmol) of potassium trimethylsilanolate. The reaction is stirred at room temperature for 18 h. The solvent is removed under reduced pressure and the residue is partitioned between water and diethyl ether. The basic aqueous layer is separated, acidified using 1M aqueous HCl solution to pH 1 and extracted with DCM (3×100 mL). The organic phase is dried over MgSO4, filtered and the filtrate is concentrated under reduced pressure to give 1.32 g of 2-(2,3-difluoro-phenylsulfanyl)-2-methyl-propionic acid as a pale yellow solid. Yield: 90%, ES-MS: m/z 231 [M−H].

WORKUP

后处理

  1. customThe solvent is removed under reduced pressure
  2. customthe residue is partitioned between water and diethyl ether
  3. customThe basic aqueous layer is separated
  4. extractionextracted with DCM (3×100 mL)
  5. dry with materialThe organic phase is dried over MgSO4
  6. filtrationfiltered
  7. concentrationthe filtrate is concentrated under reduced pressure