Reaktion #216142

ord-78beb3a0c5db426f96259fdebd22d18d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirred at room temperature for 1 hour
  2. 2
    SonstigeFurther, it is reacted at 80°-100° C. for 16 hours
  3. 3
    SonstigeAfter the completion of the reaction
  4. 4
    Waschenthe reaction solution is washed with a saline solution and further with water
  5. 5
    Trocknenthe resulting toluene layer is dried on sodium sulfate
  6. 6
    Einengenconcentrated

Vorschrift

Ethyl 2-chloro-6-fluoro-benzimidate (1.61 g) and triethylamine (1.0 g) are dissolved in toluene (100 ml), to which is added dropwise 1-methylcyclohexylcarbonyl chloride (1.5 g) at 5°-10° C. with stirring and thereafter stirred at room temperature for 1 hour. Further, it is reacted at 80°-100° C. for 16 hours. After the completion of the reaction, the reaction solution is washed with a saline solution and further with water and then the resulting toluene layer is dried on sodium sulfate and concentrated to obtain crude product of ethyl N-(1-methylcyclohexylcarbonyl)-2-chloro-6-fluorobenzimidate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05466705uspto-grants-1995_11