Reacción #2006473

ord-08b590fb32c34c1ab5e03c36feb43304

Ecuación de reacción

CC(C)(C)OP(=O)([O-])OC(C)(C)C
bis-tert butyl phosphate
ClCI
chloroiodomethane
CC(C)(C)OP(=O)(OCCl)OC(C)(C)C
di-tert-butyl chloromethyl phosphate

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe volatiles were removed in vacuo
  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 and final removal of volatiles

Procedimiento

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.

Fuente

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