Chloroiodomethane → Di-tert-butyl (chloromethyl) phosphate

HRID 20211

반응식

HRID 20211 반응식
[P:1]([O-:13])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[Cl:14][CH2:15]I>>[P:1]([O:13][CH2:15][Cl:14])([O:3][C:4]([CH3:6])([CH3:7])[CH3:5])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:2]

참가 물질

3

반응물 2

HCID 11644ChloroiodomethaneHCID 4191557Ditert-butyl phosphate

생성물 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate수율 343.6%

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c0ebcf4a032d459780495542121a9694
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745625B2

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