HRID399111
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis heated
- temperatureat reflux for 23 h
- customThe solvent was removed at reduced pressure
- additionthe residue treated with water
- extractionto extract the phosphonium salt
- extractionextracted with chloroform
- customThe phosphonium salts are crystallized from hot chloroform by addition of ethyl acetate