HRID1247390

反应详情

EQUATION

反应方程式

HRID 1247390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of (RS)-(2,6-difluoro-3-hydroxy-phenyl)-methoxy-acetic acid ethyl ester (11.6 g) and LiOH.H2O in THF (40 ml), MeOH (40 ml) and H2O was stirred 2 h at 65° C. The organic solvents were evaporated, H2O was added (50 ml) and the pH was lowered with 2 N HCl to pH=2. The product was extracted with AcOEt (3×50 ml). The organic layers were washed with brine (100 ml), combined and dried (Na2SO4). Evaporation of the solvent afforded 9.6 g (94%) of (RS)-(2,6-difluoro-3-hydroxy-phenyl)-methoxy-acetic acid. White solid. MS 217.1 ([M−H]−).

WORKUP

后处理

  1. customThe organic solvents were evaporated
  2. additionH2O was added (50 ml)
  3. extractionThe product was extracted with AcOEt (3×50 ml)
  4. washThe organic layers were washed with brine (100 ml)
  5. dry with materialdried (Na2SO4)
  6. customEvaporation of the solvent