反応 #48490

反応方程式

tetrabutylammonium di-tert-butyl phosphate

chloroiodomethane

→

di-tert-butyl chloromethyl phosphate

反応条件

後処理

1. 1
   その他were removed under vacuum
2. 2
   workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
3. 3
   ろ過was filtered away
4. 4
   その他Concentration of the filtrate in vacuo and removal of remaining volatiles

実験手順

A mixture of tetrabutylammonium di-tert-butyl phosphate (57 g, 0.126 mol, Digital Specialty Chemicals) and chloroiodomethane (221 g, 1.26 mol) was stirred at room temperature for four hours before the volatiles were removed under vacuum. 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 remaining volatiles using a vacuum pump provided di-tert-butyl chloromethyl phosphate as a light brown or yellow oil, which was utilized in the next step without further purification.

出典