Reaktion #1332016

ord-0557d641570944dcb76267f0fd976c76

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe temperature of the system was maintained at 0–5° C
  2. 2
    workup.ADDITIONabove was then added dropwise
  3. 3
    Temperaturmaintaining the reaction mixture at 0–5° C
  4. 4
    Sonstigecompletion of reaction
  5. 5
    workup.WAITAfter standing overnight at ambient temperature
  6. 6
    Einengenthe reaction mixture was concentrated at 40° C. under vacuum
  7. 7
    Trocknenfurther dried by azyeotropic distillation with toluene

Vorschrift

Ammonia gas was condensed in 2 ml water at 0–5° C. and the temperature of the system was maintained at 0–5° C. 0.68 g of methyl (2S)-2-[2-oxo-(4S)-4-propyl-1-pyrrolidinyl]butanoate obtained such as described above was then added dropwise, maintaining the reaction mixture at 0–5° C. The system was then stirred for 6 hrs, with TLC indicating completion of reaction. After standing overnight at ambient temperature the reaction mixture was concentrated at 40° C. under vacuum and further dried by azyeotropic distillation with toluene to give 150 mg of crude (2S)-2-[2-oxo-(4S)-4-propyl-1-pyrrolidinyl]butanamide.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07122682B2uspto-grants-2006_10