Reaktion #61547

ord-1eaec0aabaf74bf68499db6ce002e679

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with DCM (3×100 ml)
  2. 2
    TrocknenThe combined organic layers were dried over MgSO4
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    SonstigeThe crude product was subjected to the next reaction step without further purification

Vorschrift

To a solution of 5 g Diethyl Oxalacetate sodium salt in 100 ml ethanol, 1.5 g hydrazine monohydrochloride were added and the reaction mixture was heated to 80° C. for 3 h. Then the solution was diluted with 100 ml of water containing 3 ml of halfconcentrated HCl and extracted with DCM (3×100 ml). The combined organic layers were dried over MgSO4, filtered and concentrated under reduced pressure. The crude product was subjected to the next reaction step without further purification; Yield: 3.4 g

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429581B2uspto-grants-2008_09