Reaktion #5011

ord-d600937ba404454f851cb18c5c96b0b1

Reaktionsgleichung

CCOP(=O)(Cc1ccccc1C)OCC
diethyl 2-methylbenzylphosphonate
BrBr
Br2
CCOP(=O)(Cc1ccc(Br)cc1C)OCC
Diethyl 2-methyl-4-bromobenzylphosphonate

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONthe solution was introduced into a flask
  2. 2
    workup.STIRRINGThe mixture was stirred at 90° C. for 15 hours
  3. 3
    Temperaturafter cooling
  4. 4
    Extraktionextracted three times with 100 ml of n-hexane each time
  5. 5
    SonstigeThe organic phase wa dried
  6. 6
    Einengenconcentrated
  7. 7
    workup.DISTILLATIONdistilled

Vorschrift

10 g (42 mmol) of diethyl 2-methylbenzylphosphonate were dissolved in 60 ml of trimethyl phosphate and the solution was introduced into a flask protected from light and moisture. 16 g (0.05 mol) of Br2 were added dropwise, while stirring. The mixture was stirred at 90° C. for 15 hours and, after cooling, was diluted with 100 ml of water and extracted three times with 100 ml of n-hexane each time. The organic phase wa dried, concentrated and distilled.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05242908uspto-grants-1993_09