Chloroiodomethane → Di-tert-butyl (chloromethyl) phosphate

HRID 20210

반응식

HRID 20210 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>C1C=CC=CC=1>[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

4

반응물 2

HCID 11644ChloroiodomethaneHCID 4191557Ditert-butyl phosphate

생성물 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

The tetrabutylammonium salt of bis-tert butyl phosphate (45.1 g, 0.1 mol) and chloroiodomethane (200 g, 1.14 mol) were combined in 100 ml of benzene and the mixture was stirred at room temperature for four hours and then the benzene was removed under vacuum. A portion of 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 the volitiles on a vacuum pump provided di-tert-butyl chloromethyl phosphate, as a light yellow or light brown oil which was utilized in the next step without further purification.

후처리

  1. customthe benzene was removed under vacuum
  2. additionA portion of 500 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 the volitiles on a vacuum pump

출처 및 근거

ORD 기록
ord-13f9a7cc73b54c34b671626294596dc9
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745625B2

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