Réaction #589028

ord-ca400c4bbffe4195b8a428f6a41ceaca

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreCatalyst was removed by filtration
  2. 2
    workup.DISTILLATIONthe ethyl acetate distilled off
  3. 3
    workup.ADDITIONhexane added
  4. 4
    FiltrationThe solid product was filtered
  5. 5
    Autredried
  6. 6
    Autreto give pure 28 (0.2 g 22.8%) as a brown powder with an m.p. between 104-106.3° C.

Mode opératoire

(4—Nitrophenoxy)-acetic acid-2-hydroxyethyl ester 23 (1 g, 4.15 mmol) was dissolved in ethyl acetate in a pressure vessel. Palladium on carbon (5%, 0.5 g) was added and the mixture stirred under an atmosphere of hydrogen (0.5 kg) for one hour. Catalyst was removed by filtration, the ethyl acetate distilled off and hexane added. The solid product was filtered and dried to give pure 28 (0.2 g 22.8%) as a brown powder with an m.p. between 104-106.3° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07772352B2uspto-grants-2010_08