HRID2372978

反应详情

EQUATION

反应方程式

HRID 2372978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 15 g (33.2.10-3 mol) of 4,4'-diiodo-1,1'-biphenyl, 3.13 g (34.9.10-3 mol) of mercuric cyanide and 2.75 g (34.9.10-3 mol) of pyridine is heated at 200° C. for 15 minutes and 6 ml of dimethylformamide are then added to the mixture. After cooling, the reaction medium is hydrolyzed with a 1N aqueous solution of hydrochloric acid. The expected product is extracted with ethyl acetate. The organic phase obtained is washed with water until the pH of the washings is neutral, dried over magnesium sulfate and evaporated under vacuum. 3.28 g (yield: 33%) of a yellow solid are obtained after purification by flash chromatography using a chloroform/toluene mixture (1/1 v/v) as the eluent.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionThe expected product is extracted with ethyl acetate
  3. customThe organic phase obtained
  4. washis washed with water until the pH of the washings
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under vacuum