HRID470331

反应详情

EQUATION

反应方程式

HRID 470331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 4-bromo-o-phenylenediamine 1 (0.935 g, 5 mmol), 2-methoxy-3-pyridyl boronic acid 2 and Na2CO3 (1.060 g, 10 mmols) in 1,4-dioxane/H2O (3:1, 20 mL) flushed with N2 was added Pd(PPh3)4 (0.575 g, 0.5 mmol) in one portion. Resulting reaction mixture was stirred under N2 atmosphere at 100° C. for 12 h. Solvent was evaporated and residue was extracted with ethyl acetate (20 mL). Dried over anhydrous sodiumsulfate. Filtered, and evaporation of solvent gave a crude residue which was used as such in the following reaction. (0.850 g).

WORKUP

后处理

  1. customResulting
  2. customreaction mixture
  3. customSolvent was evaporated
  4. extractionresidue was extracted with ethyl acetate (20 mL)
  5. dry with materialDried over anhydrous sodiumsulfate
  6. filtrationFiltered
  7. customevaporation of solvent