Reaktion #64935

ord-fbb9da8152d3432bb09a0df0f86dab43

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe sodium sulphate which has precipitated
  2. 2
    Filtrationis filtered off with suction
  3. 3
    Extraktionthe filtrate is extracted with chloroform
  4. 4
    TrocknenThe extract is dried over potassium carbonate
  5. 5
    Einengenconcentrated
  6. 6
    workup.DISTILLATIONthe residue is distilled

Vorschrift

15.6 g (66mmol) of 1-benzyl-4-hydroxy-3-(2-hydroxyethylamino)-pyrrolidine are heated under reflux in a mixture of 60 ml of concentrated sulphuric acid and 20 ml of water for 6 hours. The mixture is rendered alkaline with concentrated sodium hydroxide solution, the sodium sulphate which has precipitated is filtered off with suction and the filtrate is extracted with chloroform. The extract is dried over potassium carbonate and concentrated and the residue is distilled.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05416096uspto-grants-1995_05