HRID977576

反应详情

EQUATION

反应方程式

HRID 977576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 178 mg of sodiura hydride (80% dispersion in mineral oil) in 4 ml of dimethylformamide is mixed under argon atmosphere, stirring and ice cooling with a solution of 361 mg of glycolic acid methyl ester in 2 ml of dimethylformaraide and stirred for 3 hours at room temperature. Then, a solution of 948 mg of 2,6-dibromopyridine in 2 ml of dimethylformamide is added under ice cooling and the mixture is stirred for 48 hours at room temperature. The reaction mixture is poured on ice and extracted with ethyl acetate. The organic phase is washed 4 times with saturated common salt solution, dried on sodium sulfate and concentrated by evaporation. 790 mg of 2-(6-bromo-2-pyridyloxy)acetic acid methyl ester is obtained as oily crude product.

WORKUP

后处理

  1. additionis mixed under argon atmosphere
  2. stirringthe mixture is stirred for 48 hours at room temperature
  3. additionThe reaction mixture is poured on ice
  4. extractionextracted with ethyl acetate
  5. washThe organic phase is washed 4 times with saturated common salt solution
  6. customdried on sodium sulfate
  7. concentrationconcentrated by evaporation