Chloroiodomethane → Di-tert-butyl (chloromethyl) phosphate

HRID 20212

반응식

HRID 20212 반응식
[C:1]([O:5][P:6]([O-:13])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])([CH3:4])([CH3:3])[CH3:2].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl:31][CH2:32]I>>[P:6]([O:13][CH2:32][Cl:31])([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7]

참가 물질

3

반응물 2

HCID 11644ChloroiodomethaneHCID 22339116Tetra-n-butylammonium di-tert-butylphosphate

생성물 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate

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.

후처리

  1. customwere removed under vacuum
  2. addition500 ml of ethyl ether was added to the residue and insoluble solid
  3. filtrationwas filtered away
  4. customConcentration of the filtrate in vacuo and removal of remaining volatiles

출처 및 근거

ORD 기록
ord-56a2fca1e2d24473a6fdd37fbe0d53ca
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745625B2

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