Reacción #2006474

ord-a490d813b217424c8d2caee980af7025

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowere removed under vacuum
  2. 2
    workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
  3. 3
    Filtraciónwas filtered away
  4. 4
    OtroConcentration of the filtrate in vacuo and removal of remaining volatiles

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08168615B2uspto-grants-2012_05