HRID2075498

反应详情

EQUATION

反应方程式

HRID 2075498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 1.0 g 1-hydroxy-2-naphthoic acid methyl ester in 20 ml abs. DMF 3.22 g cesium carbonate was added, followed by addition of 0.16 g potassium iodide and 0.96 g 2-chloro-5-chloromethyl-pyridine. Under argon-atmosphere the reaction mixture was heated to 60° C. for 1 h. The mixture was then poured into water and extracted with ethyl acetate at pH9 three times. The combined organic layers were dried over magnesium sulphate, filtrated and after removal of the solvent a crude product was obtained which was recrystallized from diethyl ether to yield 1.62 g 1-(6-chloro-pyridin-3-ylmethoxy)-naphthalene-2-carboxylic acid methyl ester.

WORKUP

后处理

  1. extractionextracted with ethyl acetate at pH9 three times
  2. dry with materialThe combined organic layers were dried over magnesium sulphate
  3. filtrationfiltrated
  4. customafter removal of the solvent a crude product
  5. customwas obtained which
  6. customwas recrystallized from diethyl ether