반응 #2006474

ord-a490d813b217424c8d2caee980af7025

반응 방정식

CC(C)(C)OP(=O)([O-])OC(C)(C)C.CCCC[N+](CCCC)(CCCC)CCCC
tetrabutylammonium di-tert-butyl phosphate
ClCI
chloroiodomethane
CC(C)(C)OP(=O)(OCCl)OC(C)(C)C
di-tert-butyl chloromethyl phosphate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08168615B2uspto-grants-2012_05