HRID923209

反应详情

EQUATION

反应方程式

HRID 923209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 8-(benzyloxy)-3-bromoimidazo[1,2-a]pyridine (10.0 g, 33.0 mmol), 9.39 mL (66.0 mmol) of ethynyltrimethylsilane, 0.580 g (0.825 mmol) of Pd(PPh3)2Cl2, 0.230 g (1.19 mmol) of CuI, and 5.09 mL (36.3 mmol) of diisopropylamine in 100 mL of acetonitrile was heated at reflux for 3 h under an atmosphere of N2. Upon cooling to ambient temperature, the reaction mixture was concentrated and the crude product was purified by silica gel flash chromatography (eluted with 20-50% EtOAc/hexanes) to provide 6.74 g of product: 321 m/z (M+H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 h under an atmosphere of N2
  3. concentrationthe reaction mixture was concentrated
  4. customthe crude product was purified by silica gel flash chromatography (eluted with 20-50% EtOAc/hexanes)