Réaction #59784

ord-95d4cb604fc943bdb39ab50a61f6e239

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07425638B2uspto-grants-2008_09