HRID232253

反应详情

EQUATION

反应方程式

HRID 232253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of NaOH (0.54 g, 0.013 mol) in a few ml of water was added to -2-(4-hydroxyphenoxy)propionic acid (1.22 g, 0.0067 mol) in 20 ml DMSO and the mixture was stirred for 20 minutes under N2. 5-Bromo-2,3-difluoropyridine (1.3 g, 0.0067 mol) was added and the mixture was stirred for 51/2 hours at 80°-90° C. The reaction mixture was poured into water, acidified with concentrated HCl to pH 1 and extracted into CH2Cl2. The solution was dried over Na2SO4 and the solvent was removed by rotary evaporation to yield a gum which became an off-white solid (0.78 g, 33%, M.P.94°-97° C.) upon standing.

WORKUP

后处理

  1. stirringthe mixture was stirred for 51/2 hours at 80°-90° C
  2. extractionextracted into CH2Cl2
  3. dry with materialThe solution was dried over Na2SO4
  4. customthe solvent was removed by rotary evaporation
  5. customto yield a gum which