HRID923664

反应详情

EQUATION

反应方程式

HRID 923664 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Dichlorobis(triphenylphosphine)palladium(II) (2.5 g, 3.06 mmol) is added to a mixture of 2-amino-4,6-dichloropyridine (5 g, 30.7 mmol), ethynylbenzene (7.05 g, 69 mmol), copper(I) iodide (0.58 g, 3.07 mmol), triethylamine (10.8 ml, 78 mmol), THF (25 ml) and ACN (50 ml) under argon atmosphere and is stirred at 90° C. for 17 h. The mixture is diluted with water (100 ml) and extracted with EtOAc. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by NP chromatography. Yield: 3.52 g (50%). HPLC-MS: M+H=229; tR=1.85 min (METHOD—1).

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. dry with materialThe combined organic layers are dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe product is purified by NP chromatography