Reaktion #2205725

Reaktionsgleichung

methyl 2-oxo-1-pyrrolidineacetate

7a-(aminomethyl)pyrrolizidine

hydrochloric acid

→

desired compound

7a-(2-oxo-1-pyrrolidineacetamidomethyl)pyrrolizidine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   TemperaturAfter cooling
3. 3
   Extraktionextracted 3 times with dichloromethane
4. 4
   workup.ADDITIONby the addition of sodium hydroxide solution
5. 5
   Extraktionextracted 3 times with dichloromethane
6. 6
   Trocknenby drying over anhydrous magnesium sulfate
7. 7
   SonstigeAfter removal of the drying agent
8. 8
   Filtrationthrough filtration
9. 9
   Sonstigethe solvent was evaporated under reduced pressure

Vorschrift

A mixture consisting of 14.1 g (89.6 mmol) of methyl 2-oxo-1-pyrrolidineacetate and 11.4 g (81.4 mmol) of 7a-(aminomethyl)pyrrolizidine was heated and stirred for 6 hours at 80° C. under argon atmospher. After cooling, the reaction mixture was then solved with 1.0N-hydrochloric acid and extracted 3 times with dichloromethane. An aqueous layer was rendered alkaline by the addition of sodium hydroxide solution and extracted 3 times with dichloromethane followed by drying over anhydrous magnesium sulfate. After removal of the drying agent through filtration, the solvent was evaporated under reduced pressure to obtain a yellowish oil as a free base of the desired compound. The free base was converted to terephthalate by usual manner. Yield: 32.0 g (91.1%).

Quelle