HRID232253
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringthe mixture was stirred for 51/2 hours at 80°-90° C
- extractionextracted into CH2Cl2
- dry with materialThe solution was dried over Na2SO4
- customthe solvent was removed by rotary evaporation
- customto yield a gum which