HRID364647

反应详情

EQUATION

反应方程式

HRID 364647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

There is prepared from 50 g triphenylphosphine and 38.5 g 1,3-dibrompropane in 150 ml xylene by heating for 20 hours at 130° C. under nitrogen 80 g crystalline (3-bromopropyl)-triphenylphosphoniumbromide with a melting point of 226° C. This is stirred using a solution of 33 g (0.7M) dimethylamine in 200 ml ethanol for 20 hours at 20°-25° C.) The residue is absorbed after removal of ethanol in a vacuum in 2-propanol and precipitated using hydrogen bromide gas. After recrystallization from ethanol, 43 g (3-dimethylaminopropyl)-triphenylphosphoniumbromide HBr is obtained with a melting point of 279° C.

WORKUP

后处理

  1. customfor 20 hours
  2. customat 20°-25° C.
  3. customis absorbed
  4. customafter removal of ethanol in a vacuum in 2-propanol
  5. customprecipitated
  6. customAfter recrystallization from ethanol