HRID399111

反应详情

EQUATION

反应方程式

HRID 399111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A mixture of hydroxymethyl)triphenylphosphonium bromide and phosphorus tribromide in benzene is heated at reflux for 23 h with stirring. After this time the solution is dark orange and an orange solid is present. The mixture is cooled to 25° C. and methanol is added. The solvent was removed at reduced pressure and the residue treated with water to extract the phosphonium salt. The aqueous extracts were saturated with solid potassium bromide and extracted with chloroform. The phosphonium salts are crystallized from hot chloroform by addition of ethyl acetate.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux for 23 h
  3. customThe solvent was removed at reduced pressure
  4. additionthe residue treated with water
  5. extractionto extract the phosphonium salt
  6. extractionextracted with chloroform
  7. customThe phosphonium salts are crystallized from hot chloroform by addition of ethyl acetate