Reaktion #48490

ord-56a2fca1e2d24473a6fdd37fbe0d53ca

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewere removed under vacuum
  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 in vacuo and removal of remaining volatiles

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745625B2uspto-grants-2010_06