Reaktion #1500296

ord-1cd372f57d2144c7a99f3865a3f5bcee

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is then refluxed
  2. 2
    workup.STIRRINGAfter having stirred for 2 hours at the ambient temperature
  3. 3
    Sonstigethe precipitate formed
  4. 4
    Sonstigeis separated by filtration
  5. 5
    SonstigeThe filtrate obtained
  6. 6
    Trocknenis dried over magnesium sulfate
  7. 7
    workup.DISTILLATIONthe solvent is distilled under reduced pressure

Vorschrift

65.6 g of 5-benzoyl-2-pyrrolidone prepared as indicated in above part (a) are added in small fractions, under a nitrogen atmosphere, to a suspension of 26.4 g of lithium aluminium hydride in 4 liters of anhydrous tetrahydrofuran. The mixture is then refluxed with stirring for 2 hours. It is then cooled to 0° C. and then are slowly added 30.5 ml of water, then 11 ml of a 10 N solution of sodium hydroxide and finally 110 ml of water. After having stirred for 2 hours at the ambient temperature, the precipitate formed is separated by filtration. The filtrate obtained is dried over magnesium sulfate and the solvent is distilled under reduced pressure. 53 g of α-phenyl-2-pyrrolidine methanol are obtained. These 53 g are recrystallized from 580 ml of isopropyl ether. 36 g of α-phenyl-2-pyrrolidine methanol (erythro) melting at 110° C. are thus obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04248884uspto-grants-1981_02