HRID983414

反应详情

EQUATION

反应方程式

HRID 983414 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 6-bromo-3-methoxy-pyridine-2-carbonitrile from Example 13c in toluene is treated with 2 M Na2CO3 (aqueous), 4-carboxylphenylboronic acid (1 equiv.), ethanol and catalytic (Ph3P)4Pd) and is heated at 80° C. for 18 h. The reaction mixture is evaporated and the residue is dissolved in ethanol with 4 N HCl in dioxane and heated at reflux for 18 h. The reaction mixture is evaporated, the residue taken into ethyl acetate, washed with 5% Na2CO3 (aqueous), dried over MgSO4 and evaporated to give 4-(6-cyano-5-methoxy-pyridin-2-yl)-benzoic acid ethyl ester.

WORKUP

后处理

  1. customThe reaction mixture is evaporated
  2. dissolutionthe residue is dissolved in ethanol with 4 N HCl in dioxane
  3. temperatureheated
  4. temperatureat reflux for 18 h
  5. customThe reaction mixture is evaporated
  6. washwashed with 5% Na2CO3 (aqueous)
  7. dry with materialdried over MgSO4
  8. customevaporated