Reacción #67706

ord-98c6ae645cf442be9c235d2382fa39de

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturarefluxed for 10 min
  2. 2
    TemperaturaThe reaction mixture was refluxed for 2 h
  3. 3
    OtroThe reaction mixture was quenched with 8 mL water
  4. 4
    Filtraciónfiltered through dicalite
  5. 5
    OtroThe organic phase was separated
  6. 6
    Otrodried on sodium sulfate
  7. 7
    Filtraciónfiltered
  8. 8
    Otroevaporated
  9. 9
    OtroThe crude material, brown oil (3.54 g, 82%) was used without further purification

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08524909B2uspto-grants-2013_09