Reaktion #549902

ord-85922ff6c0a746a3b35fa11c48dc64ca

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITwas left under agitation for an hour at room temperature
  2. 2
    ExtraktionThen it was extracted with methylene chloride
  3. 3
    Filtrationfiltered
  4. 4
    Waschenthe filtrate was washed with water
  5. 5
    Sonstigedried on sodium sulfate
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigethe filtrate was evaporated
  8. 8
    Sonstigethe residue crystallized in a mixture of ethyl acetate and isopropylic ether

Vorschrift

A mixture of 23 g of formula (IX) compound obtained in the preceding example and 23 g of powdered iron in 200 ml of an aqueous solution of 10% ammonium chloride and 20 ml of ethanol was left under agitation for an hour at room temperature. Then it was extracted with methylene chloride, filtered, the filtrate was washed with water, dried on sodium sulfate, filtered, the filtrate was evaporated and the residue crystallized in a mixture of ethyl acetate and isopropylic ether. 18.6 g of the expected compound were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04517197uspto-grants-1985_05