HRID76170

反应详情

EQUATION

反应方程式

HRID 76170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

24.6 g (168 mmol) 1-ethoxy-4-ethynyl-benzene, 52.8 g (176 mmol) [1-(4-Bromo-phenyl)-ethyl]-carbamic acid tert-butyl ester (50.2) and 42.6 mL (307 mmol) TEA are added to 400 mL ACN. The mixture is warmed to 65° C. 8.84 g (7.65 mmol) Pd(PPh3)4 and 2.91 g (15.3 mmol) CuI are added and the reaction mixture is stirred at reflux for 2 h. The mixture is cooled to r.t. and the solvent is removed in vacuo. The crude product is purified by column chromatography (hexane/EtOAC 9:1→3:1).

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. temperatureThe mixture is cooled to r.t.
  3. customthe solvent is removed in vacuo
  4. customThe crude product is purified by column chromatography (hexane/EtOAC 9:1→3:1)