Reaktion #56534

ord-ba867d69358d4678ae07e3c7210e9ee7

Lösungsmittel

Reaktionsbedingungen

Temperatur
135°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis heated
  2. 2
    Extraktionextracted with ether
  3. 3
    TrocknenThe combined ether extracts are dried over magnesium sulfate
  4. 4
    FiltrationThe drying agent is filtered and into the ethereal solution
  5. 5
    Sonstigeis bubbled dry hydrogen chloride gas
  6. 6
    SonstigeThe white solid which precipitates
  7. 7
    Sonstigeis collected
  8. 8
    Sonstigedried
  9. 9
    Sonstigeto give 70.4 g

Vorschrift

A mixture of 2-cyano-2-(2,4-dichlorophenyl)hexyl methane sulfonate (100 g., 0.29 mole), imidazole (100 g., 1.5 mole) and N,N-dimethylformamide (5 ml.) is heated with stirring at 135° C. overnight. The reaction mixture is poured into water and extracted with ether. The combined ether extracts are dried over magnesium sulfate. The drying agent is filtered and into the ethereal solution is bubbled dry hydrogen chloride gas. The white solid which precipitates is collected and dried to give 70.4 g. (68%) of the expected product, which is identified by nmr.

Quelle

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