Reaktion #56546

ord-01d526c28d0343faaf6133d71910b692

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ether
  2. 2
    TrocknenThe combined ether extracts are dried over magnesium sulfate
  3. 3
    Filtrationfiltered
  4. 4
    SonstigeInto the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms
  5. 5
    SonstigeThe solvent is then decanted
  6. 6
    ExtraktionThe purified free base is extracted into ether
  7. 7
    Trocknendried over magnesium sulfate
  8. 8
    SonstigeWhen the solvent is evaporated

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225723uspto-grants-1980_09