Reacción #56546

ord-01d526c28d0343faaf6133d71910b692

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextracted with ether
  2. 2
    SecadoThe combined ether extracts are dried over magnesium sulfate
  3. 3
    Filtraciónfiltered
  4. 4
    OtroInto the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms
  5. 5
    OtroThe solvent is then decanted
  6. 6
    ExtracciónThe purified free base is extracted into ether
  7. 7
    Secadodried over magnesium sulfate
  8. 8
    OtroWhen the solvent is evaporated

Procedimiento

A mixture of 6-cyano-6-(2,4-dichlorophenyl)decyl bromide (14.2g., 0.036 mole) imidazole (10g., 0.15 mole) and 5 ml. N,N-dimethylformamide is heated at 120° C. for 24 hours. The reaction mixture is poured into water and extracted with ether. The combined ether extracts are dried over magnesium sulfate and filtered. Into the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms. The solvent is then decanted and the oily residue is taken up in acetone and neutralized with dilute ammonium hydroxide solution. The purified free base is extracted into ether and dried over magnesium sulfate. When the solvent is evaporated, a total of 6.5 g. (47.8%) of product is obtained, which is identified by nmr.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04225723uspto-grants-1980_09