Reaktion #472195

ord-d155db9a08a245189aab07163777c986

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture was extracted with ethyl acetate
  2. 2
    WaschenThe organic layer was washed with 1N hydrochloric acid and saturated brine
  3. 3
    Trocknendried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

5-bromo-2-hydroxy-3-trifluoromethylbenzaldehyde (63.98 g) was dissolved in N,N-dimethylformamide (130 mL), and potassium carbonate (65.79 g) and dimethylsulfuric acid (31.6 mL) were added to the solution under water cooling, and then the mixture was stirred at room temperature for 3 hours. Water was added to the reaction solution, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (66.19 g) as a brown crystal.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08367843B2uspto-grants-2013_02