Reaktion #1332016
ord-0557d641570944dcb76267f0fd976c76
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturthe temperature of the system was maintained at 0–5° C
- 2workup.ADDITIONabove was then added dropwise
- 3Temperaturmaintaining the reaction mixture at 0–5° C
- 4Sonstigecompletion of reaction
- 5workup.WAITAfter standing overnight at ambient temperature
- 6Einengenthe reaction mixture was concentrated at 40° C. under vacuum
- 7Trocknenfurther 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.