反应 #48488

反应方程式

bis-tert butyl phosphate

chloroiodomethane

→

di-tert-butyl chloromethyl phosphate

溶剂

benzene

反应条件

后处理

1. 1
   其他the benzene was removed under vacuum
2. 2
   workup.ADDITIONA portion of 500 ml of ethyl ether was added to the residue and insoluble solid
3. 3
   过滤was filtered away
4. 4
   其他Concentration of the filtrate in vacuo and removal of the volitiles on a vacuum pump

实验过程

The tetrabutylammonium salt of bis-tert butyl phosphate (45.1 g, 0.1 mol) and chloroiodomethane (200 g, 1.14 mol) were combined in 100 ml of benzene and the mixture was stirred at room temperature for four hours and then the benzene was removed under vacuum. A portion of 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate in vacuo and removal of the volitiles on a vacuum pump provided di-tert-butyl chloromethyl phosphate, as a light yellow or light brown oil which was utilized in the next step without further purification.

来源