HRID1484912

反应详情

EQUATION

反应方程式

HRID 1484912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

Under nitrogen atmosphere, a mixture of 2,4-dichloro-5-iodopyrimidine (2.0 g, 7.3 mmol, 1.0 eq), Pd(PPh3)2Cl2 (256 mg, 0.37 mmol, 0.05 eq), CuI (139 mg, 0.73 mmol, 0.1 eq) Et3N (2.2 g, 21.9 mmol, 3.0 eq) and ethynyltrimethylsilane (1.4 g, 14.6 mmol, 1.2 eq) in THF (20 ml) was stirred at 35° C. for 4 h. The mixture was filtered and concentrated. The residue was purified by silica gel column chromatography (PE/EtOAc=200:1) to give compound 2,4-dichloro-5-((trimethylsilyl)ethynyl)pyrimidine (1.0 g, 56%).

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customThe residue was purified by silica gel column chromatography (PE/EtOAc=200:1)