HRID351445

反应详情

EQUATION

反应方程式

HRID 351445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To the solution of 4-methoxy-phenyl-acetylene (10 g, 0.075 mol) and 4-iodo-anisole (17.65 g, 1.0 eq.) in diethylamine (150 mL) was added Pd(PPh3)2Cl2 (2.65 g, 0.05 eq.) and the reaction mixture was stirred for 30 min at 0° C. To the reaction mixture was then added Cul (1.43 g, 0.1 eq.) and the mixture was stirred at 6 h at 0˜25° C. The reaction mixture was then concentrated and partitioned between ethyl acetate/H2O (200/600 mL). The organic layer was separated, dried and purified on SiO2 (1˜5% ethyl acetate/hexane) to yield 1,2-di(4-methoxy-phenyl)-acetylene.

WORKUP

后处理

  1. stirringadded Cul (1.43 g, 0.1 eq.) and the mixture was stirred at 6 h at 0˜25° C
  2. concentrationThe reaction mixture was then concentrated
  3. custompartitioned between ethyl acetate/H2O (200/600 mL)
  4. customThe organic layer was separated
  5. customdried
  6. custompurified on SiO2 (1˜5% ethyl acetate/hexane)