Reaktion #564042

ord-1b83a84a119a4bdfaf4b63abc32196be

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONhad been added
  2. 2
    workup.WAITThe mixture was left overnight at room temperature
  3. 3
    workup.STIRRINGunder stirring for 2 hours
  4. 4
    SonstigeThe mixture was then evaporated
  5. 5
    Sonstigethe residue was partitioned between diethylether and water
  6. 6
    SonstigeThe organic phase was evaporated

Vorschrift

20 g o-nitro benzylalcohol and 21.7 ml ethyl bromoacetate was dissolved in 250 ml dry DMF. Portions of 55-60% sodium hydride were added to this solution under stirring over one hour until a total amount of 8.5 g had been added. The mixture was left overnight at room temperature and then heated to 150° C. under stirring for 2 hours. The mixture was then evaporated and the residue was partitioned between diethylether and water. The organic phase was evaporated to give 14 g ethyl (o-nitro-benzyloxy)acetate as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04886797uspto-grants-1989_12