Dimethylformamide dimethyl acetal → (Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate
Reaktionsgleichung
[O:1]=[C:2]1[CH2:6][CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:3]1.[CH3:14][N:15]([CH:17](OC)OC)[CH3:16]>>[CH3:14][N:15](/[CH:17]=[C:6]1/[CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:3][C:2]/1=[O:1])[CH3:16]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 105 °C
Versuchsvorschrift
A solution of tert-butyl 3-oxopyrrolidine-1-carboxylate (40 g, 216 mmol) was treated with DMF-DMA (267 g, 2241 mmol) and heated at 105° C. for 40 min. The solution was cooled and evaporated under reduced pressure and the resulting orange solid was treated with hexane (200 mL) and cooled in the refrigerator over the weekend. The resulting brownish-yellow solid was collected by filtration, dried and used in the next setp without further purification.
Aufarbeitung
- temperatureThe solution was cooled
- customevaporated under reduced pressure
- additionthe resulting orange solid was treated with hexane (200 mL)
- temperaturecooled in the refrigerator over the weekend
- filtrationThe resulting brownish-yellow solid was collected by filtration
- customdried
- customused in the next setp without further purification
Quellen und Nachweise
- ORD-Eintrag
- ord-11d731c7e4c64484b49ae2a720346b76
- Quelldatensatz
- uspto-grants-2010_03
- Patentnummer
- US07678905B2
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