Reaktion #67706

ord-98c6ae645cf442be9c235d2382fa39de

Reaktionsgleichung

BrC1CC1
Cyclopropylbromide
[Mg]
magnesium
CCCCN=Cc1c(F)cc(C(F)(F)F)cc1C(F)(F)F
butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine
CCCCN=Cc1c(F)cc(C(F)(F)F)cc1C(F)(F)F
intermediate M
CCCCN=Cc1c(F)cc(C(F)(F)F)cc1C(F)(F)F
butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine
CCCCN=Cc1c(C2CC2)cc(C(F)(F)F)cc1C(F)(F)F
Butyl-[1-(2-cyclopropyl-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 10 min
  2. 2
    TemperaturThe reaction mixture was refluxed for 2 h
  3. 3
    SonstigeThe reaction mixture was quenched with 8 mL water
  4. 4
    Filtrationfiltered through dicalite
  5. 5
    SonstigeThe organic phase was separated
  6. 6
    Sonstigedried on sodium sulfate
  7. 7
    Filtrationfiltered
  8. 8
    Sonstigeevaporated
  9. 9
    SonstigeThe crude material, brown oil (3.54 g, 82%) was used without further purification

Vorschrift

Cyclopropylbromide (3.84 g, 32 mmol) was added to magnesium (771 mg, 32 mmol) in 20 mL diethylether and refluxed for 10 min. Manganese(II) chloride (160 mg, 1.27 mmol) and butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine (intermediate M, 4 g, 13 mmol) was added. The reaction mixture was refluxed for 2 h. The reaction mixture was quenched with 8 mL water and filtered through dicalite. The organic phase was separated and dried on sodium sulfate, filtered and evaporated. The crude material, brown oil (3.54 g, 82%) was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524909B2uspto-grants-2013_09