Reaktion #8539

ord-11ea0b2a940b4be2882a47ea40b946fa

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat 0° C
  2. 2
    Sonstigethe solvent was evaporated
  3. 3
    workup.ADDITIONAfter adding water
  4. 4
    Waschenthe 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
    ExtraktionThen the aqueous layer was extracted with IPE
  7. 7
    TrocknenThe organic layer was dried over anhydrous magnesium sulfate
  8. 8
    Sonstigethe solvent was evaporated

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087778B2uspto-grants-2006_08