HRID470917

反应详情

EQUATION

反应方程式

HRID 470917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A three neck flask was charged with 250 g of m-terphenyl (manufactured by Aldrich Co., Ltd.), 50 g of hydroiodic acid dihydrate, 75 g of iodine, 750 mL of acetic acid and 25 mL of cone, sulfuric acid, and they were reacted at 70° C. for 3 hours. After reaction, the solution was poured into 5 L of methanol and then stirred for one hour. This was separated by filtration, and crystal obtained was refined by means of column chromatography and recrystallized from acetonitrile to obtain 64 g of 5-phenyl-3-iodobiphenyl (intermediate 3) shown, below and 17 g of 3′-phenyl-4-iodobiphenyl (intermediate 4) shown below.

WORKUP

后处理

  1. customwere reacted at 70° C. for 3 hours
  2. customAfter reaction
  3. customThis was separated by filtration, and crystal
  4. customobtained
  5. customrecrystallized from acetonitrile