Reaktion #417188

ord-00d49b3b9b81425a964f7c543b421b03

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwere added to the resulting solution, whilst ice-
  2. 2
    Temperaturcooling
  3. 3
    workup.ADDITIONwas added to the resulting mixture
  4. 4
    TemperaturThe mixture was then heated at 70° to 75° C. for 2.5 hours
  5. 5
    workup.ADDITIONAt the end of this time, the resulting mixture was treated
  6. 6
    Sonstigepurified similarly to the procedure

Vorschrift

965 mg of methyl 4-mercaptobenzoate were dissolved in 6 ml of dry dimethylformamide. 250 mg of a 55% w/w suspension of sodium hydride in mineral oil were added to the resulting solution, whilst ice-cooling, and the mixture was then stirred at room temperature for 30 minutes. A solution of 1.1 g of 1-[2-chloro-2-(4-fluorophenyl)ethyl]imidazole dissolved in 16 ml of dry dimethylformamide was added to the resulting mixture. The mixture was then heated at 70° to 75° C. for 2.5 hours. At the end of this time, the resulting mixture was treated and purified similarly to the procedure described in Example 1, to give 866 mg of the title compound as a powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04894385uspto-grants-1990_01