Reaktion #410853

ord-89cbb5de9fa948c39df2c25e5c23821f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas slowly added dropwise
  2. 2
    Extraktionextracted twice with 150 ml of diethyl ether
  3. 3
    Waschenwashed with water
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    Einengenconcentrated
  6. 6
    Sonstigeto give a crude product

Vorschrift

A reaction vessel was charged with 10.6 g of 1,3-dibromopropane, 5.53 g of potassium carbonate and 100 ml of N,N-dimethylformamide, and a solution of 10.1 g of 2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenol dissolved in 40 ml of N,N-dimethylformamide was slowly added dropwise. After stirring at room temperature for 24 hours, the reaction mixture was poured into water and extracted twice with 150 ml of diethyl ether. The ether layers were combined, washed with water, dried over anhydrous magnesium sulfate, and then concentrated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 11.1 g of 3,5-dichloro-4-(3-bromopropoxy)-1-(3,3-dichloro-2-propenyloxy)benzene (77% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06214835B1uspto-grants-2001_04