HRID1388545

反应详情

EQUATION

反应方程式

HRID 1388545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 41.6 g of phosphorus tribromide, 25 ml of benzene and 8.2 ml of pyridine is prepared while cooling and while stirring it is treated dropwise at a maximum temperature of 10° C. with 108.3 g of 5-chloro-2-iodobenzyl alcohol. Then, it is stirred for 4 hours at room temperature and for 1 hour at 50° C. After cooling, it is diluted with 120 ml of chloroform, the mixture washed with 25 ml of 5% hydrochloric acid, a 5% sodium hydroxide solution and with water, dried with magnesium sulfate and evaporated. There are obtained 126 g (95%) of crude 5-chloro-2-iodobenzyl bromide melting at 75°-79° C. The pure product is obtained by crystallization from a mixture of benzene and petroleum ether, m.p. 77°-79° C.

WORKUP

后处理

  1. customis prepared
  2. temperaturewhile cooling
  3. stirringThen, it is stirred for 4 hours at room temperature and for 1 hour at 50° C
  4. temperatureAfter cooling
  5. washthe mixture washed with 25 ml of 5% hydrochloric acid
  6. dry with materiala 5% sodium hydroxide solution and with water, dried with magnesium sulfate
  7. customevaporated