Réaction #8539

ord-11ea0b2a940b4be2882a47ea40b946fa

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 IPE
  7. 7
    SéchageThe organic layer was dried over anhydrous magnesium sulfate
  8. 8
    Autrethe solvent was evaporated

Mode opératoire

Ethyl 2-(2,3,4-trifluoroanilino)propionate (2.47 g) was dissolved in ethanol (40 ml) and an aqueous solution (3 mol/l; 10 ml) of sodium 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 IPE. The organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated to give the title compound (2.19 g) as colorless crystals. Various spectral data of this product was identical with those obtained in Example 23.

Source

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