Reaktion #53557

ord-6874889d9b6847a0840fc9cf974c3a49

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting reaction mixture
  2. 2
    Extraktionextracted with 50 ml of ethyl acetate twice
  3. 3
    WaschenThe ethyl acetate layer was washed with 50 ml of water twice
  4. 4
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
  5. 5
    SonstigePurification of the residue by silica gel column chromatography

Vorschrift

3.3 g (4.9 mmol) of 1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene], 3.0 g (19.5 mmol) of Rongalite and 3.0 g (17.6 mmol) of isopropyl iodide were stirred in 30 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dtied over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.4 g of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylphenyl] isopropyl sulfide (yield 38.0%) as a yellow dough (nD20 1.5462).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858639B2uspto-grants-2005_02