Reaktion #83765

ord-73f060dfe6de4044aca39bfe30d68e8e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONAt the end of this time, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure
  2. 2
    SonstigeThe residue thus obtained
  3. 3
    Extraktionafter which it was extracted with ethyl acetate
  4. 4
    WaschenThe extract was washed with water
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    Sonstigeafter which the solvent was removed by distillation under reduced pressure
  7. 7
    SonstigeThe resulting residue was crystallized by trituration with hexane

Vorschrift

A solution of 56 g of 4-nitrophenol, 90 g of methyl bromoacetate and 100 g of potassium carbonate in 500 ml of dimethylformamide was stirred at room temperature for 2 days. At the end of this time, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure. The residue thus obtained was diluted with water, after which it was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The resulting residue was crystallized by trituration with hexane, to give 63.3 g of the title compound, melting at 98°-99° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05624935uspto-grants-1997_04