Reaktion #59784

ord-95d4cb604fc943bdb39ab50a61f6e239

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITThe progress of the reaction was checked every few days
  2. 2
    SonstigeNitrogen gas was bubbled through the solution
  3. 3
    Sonstigeto remove excess hydrogen chloride gas
  4. 4
    SonstigeThe solvent was removed
  5. 5
    Sonstigethe residue was triturated in diethyl ether

Vorschrift

2-Ethoxy-4-trifluoromethyl-benzonitrile (64 g) was dissolved in 750 mL of anhydrous ethanol. The solution was cooled to 0° C. and saturated with hydrogen chloride gas. The reaction flask was then sealed with a Teflon stopper and stirred at room temperature for 11 d. The progress of the reaction was checked every few days, and the solution was saturated again with hydrogen chloride gas. Nitrogen gas was bubbled through the solution to remove excess hydrogen chloride gas. The solvent was removed and the residue was triturated in diethyl ether to afford ethyl 2-ethoxy-4-trifluoromethyl-benzimidate hydrochloride (59.5 g, 67% yield) as white solids.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425638B2uspto-grants-2008_09