Reacción #998442

ord-79e0bde105334bc1a6a905e6f12bbecf

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheat
  2. 2
    Temperaturaat reflux for 48 h
  3. 3
    Filtraciónfilter
  4. 4
    Otroevaporate
  5. 5
    OtroPurify by chromatography on silica gel eluting with hexane/EtOAc (10 and 9:1)

Procedimiento

Mix 4-cyanophenol (1.2 g, 10 mmol), 1-bromo-3,3-dimethylbutane (5.3 g, 32 mmol), powdered potassium carbonate (4.14 g, 30 mmol), and powdered potassium iodide (166 mg, 1 mmol) in acetone (60 mL). Stir under inert atmosphere and heat at reflux for 48 h. Cool the reaction mixture to ambient temperature. Dilute with acetone, filter and evaporate. Purify by chromatography on silica gel eluting with hexane/EtOAc (10 and 9:1) to obtain the desired intermediate (1.8 g, 89%). MS (ES+) m/z: 221 (M+NH4)+.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08022062B2uspto-grants-2011_09