Reaktion #48489

Reaktionsgleichung

bis-tert butyl phosphate

chloroiodomethane

→

di-tert-butyl chloromethyl phosphate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe volatiles were removed in vacuo
2. 2
   workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
3. 3
   Filtrationwas filtered away
4. 4
   SonstigeConcentration of the filtrate and final removal of volatiles

Vorschrift

The tetrabutylammonium salt of bis-tert butyl phosphate (57 g, 0.126 mol, Digital Specialty Chemicals) and chloroiodomethane (221 g, 1.26 mol) were stirred at room temperature for four hours and then the volatiles were removed in vacuo. 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate and final removal of volatiles using a vacuum pump provided di-tert-butyl chloromethyl phosphate (112 g), typically as a light yellow or brown oil, which was utilized in the next step without any further purification.

Quelle