Réaction #8538

ord-8b10cb0936e1470cb7743fcc2219590f

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autreat 0° C
  2. 2
    Autrethe solvent was evaporated
  3. 3
    workup.ADDITIONAfter adding water
  4. 4
    Lavagethe residue was washed with chloroform
  5. 5
    workup.ADDITIONNext, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value
  6. 6
    ExtractionThen the aqueous layer was extracted with diisopropyl ether (IPE)
  7. 7
    SéchageThe organic layer was dried over anhydrous magnesium sulfate
  8. 8
    Autrethe solvent was evaporated

Mode opératoire

Methyl 2-(2,3,4-trifluoroanilino)propionate (46.64 g) was dissolved in methanol (130 ml) and an aqueous solution (3 mol/l; 100 ml) of lithium hydroxide was slowly added thereto at 0° C. After stirring at room temperature for 3 hours, the solvent was evaporated. After adding water, the residue was washed with chloroform. Next, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value reached 1. Then the aqueous layer was extracted with diisopropyl ether (IPE). The organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated to give the title compound (43.7 g) as colorless crystals.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07087778B2uspto-grants-2006_08