Reacción #472254

ord-ac9ea6db15354d0495242363ade9a0de

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.DISTILLATIONThe organic solvent was distilled off under reduced pressure
  2. 2
    Lavadothe aqueous layer was washed with n-hexane
  3. 3
    Extracciónextracted with ethyl acetate
  4. 4
    LavadoThe organic layer was washed with saturated brine
  5. 5
    Secadodried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Procedimiento

Methyl 3-cyano-5-iodo-4-methoxybenzoate (8.00 g) was dissolved in tetrahydrofuran (100 mL) and water (50 mL), and lithium hydroxide monohydrate (423 g) was added to the solution, and then the mixture was stirred at room temperature for 4 hours. The organic solvent was distilled off under reduced pressure and the aqueous layer was washed with n-hexane. The aqueous layer was acidified with 2N hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (7.26 g) as a colorless crystal.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08367843B2uspto-grants-2013_02