Chloroiodomethane → Di-tert-butyl (chloromethyl) phosphate

HRID 20211

Reaktionsgleichung

Reaktionsgleichung von HRID 20211
[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]

Komponenten

3

Edukt 2

HCID 11644ChloroiodomethaneHCID 4191557Ditert-butyl phosphate

Produkt 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphateAusbeute 343,6 %

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-c0ebcf4a032d459780495542121a9694
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07745625B2

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