Reaktion #82799

ord-e44dbfde469446e78ff3839f598915a5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis heated
  2. 2
    Temperaturunder reflux for 16 hours
  3. 3
    Temperaturcooled
  4. 4
    workup.ADDITIONpoured onto ice-dilute hydrochloric acid
  5. 5
    Extraktionextracted with dichloromethane
  6. 6
    SonstigeThe extract is dried
  7. 7
    Sonstigeevaporated
  8. 8
    Sonstigethe residue is crystallized from ether-hexane as pale crystals, m.p. <50° C.

Vorschrift

A stirred mixture of 2-nitrophenol (13.9 g, 0.10 mol), benzyl bromide (12.0 ml, 0.10 mol) and anhydrous potassium carbonate (30 g, 0.22 mol) in acetone (200 ml) is heated under reflux for 16 hours, cooled, poured onto ice-dilute hydrochloric acid, and extracted with dichloromethane. The extract is dried and evaporated and the residue is crystallized from ether-hexane as pale crystals, m.p. <50° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05622969uspto-grants-1997_04