Reaktion #572394

ord-b88dff0518304b6cb9e09dd84813d456

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of 17.4 g
  2. 2
    workup.DISTILLATIONthe solvent was distilled off
  3. 3
    workup.ADDITION2N-HCl was added to the residue
  4. 4
    Sonstigeto obtain a crude crystal
  5. 5
    SonstigeThe product was separated by a filtration
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigedried
  8. 8
    Sonstigerecrystallized from n-hexane
  9. 9
    Sonstigeto obtain 27.4 g

Vorschrift

A mixture of 17.4 g. of 2-chloro-5-nitrophenol, 19.0 g. of ethyl α-bromopropionate, 15.2 g. of potassium carbonate and 85 ml. of acetone was refluxed with stirring for 3.5 hours and the solvent was distilled off. 2N-HCl was added to the residue to obtain a crude crystal. The product was separated by a filtration and washed with water and dried and recrystallized from n-hexane to obtain 27.4 g. of the object compound (melting point of 46° to 46.5° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04536209uspto-grants-1985_08