반응 #59784

ord-95d4cb604fc943bdb39ab50a61f6e239

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425638B2uspto-grants-2008_09