Dimethylformamide dimethyl acetal → (Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate

HRID 2244572Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2244572
[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

  1. temperatureThe solution was cooled
  2. customevaporated under reduced pressure
  3. additionthe resulting orange solid was treated with hexane (200 mL)
  4. temperaturecooled in the refrigerator over the weekend
  5. filtrationThe resulting brownish-yellow solid was collected by filtration
  6. customdried
  7. 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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