Ammonium Hydroxide → 3-Cyclohexylpyrrolidin-2-one

HRID 1670812Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1670812
[CH:1]1([CH:7]2[CH2:11][CH2:10][O:9][C:8]2=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[NH4+:14]>C(O)C>[CH:1]1([CH:7]2[CH2:11][CH2:10][NH:14][C:8]2=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 14923Ammonium HydroxideHCID 220132343-Cyclohexyl-dihydro-furan-2-one

Produkt 1

HCID 576579993-Cyclohexylpyrrolidin-2-oneAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Heat a mixture of 3-cyclohexyl-dihydro-furan-2-one (32.2 g), ammonium hydroxide (700 mL) and ethanol (700 mL) at 230° C. in a sealed steel bottle for 18 hours. Cool the reaction and remove the solvent in vacuo. Partition the residue with ethyl acetate (500 mL) and HCl (1N, 300 mL). Dry the organic over sodium sulfate. After filtration and concentration, recrystallize with 1:3 ethyl acetate:hexane to afford 30 grams (94%) of the title compound.

Aufarbeitung

  1. temperatureHeat
  2. temperatureCool
  3. customthe reaction
  4. customremove the solvent in vacuo
  5. customPartition the residue with ethyl acetate (500 mL) and HCl (1N, 300 mL)
  6. dry with materialDry the organic over sodium sulfate
  7. filtrationAfter filtration and concentration
  8. customrecrystallize with 1:3 ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c2deaf126d1e4c1a91c00912e7ccb0ee
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07994176B2

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