Potassium Carbonate → HCID 178451986, Verbindung

HRID 1408339Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1408339
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]#[N:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])([O-])=O.[K+].[K+].Cl.[NH2:23][OH:24]>O.CCO>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[NH:15])[NH:23][OH:24])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 1514443Tert-butyl 4-cyanopiperidine-1-carboxylate

Produkt 1

HCID 178451986HCID 178451986, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of 4-cyano-piperidine-1-carboxylic acid tert-butyl ester (6.3 g, 30 mmol), K2CO3 (4.2 g, 30 mmol) in H2O (50 mL) and EtOH (30 mL) was added hydroxylamine hydrogenchloride (4.17 g, 60 mmol). The mixture was heated under reflux overnight, cooled to room temperature and ethanol was removed in vacuo. The residue was extracted with EtOAc (300 mL). The organic layer was washed successively with H2O and brine. After drying (Na2SO4), the solvent was removed to afford the desired product.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux overnight
  3. customethanol was removed in vacuo
  4. extractionThe residue was extracted with EtOAc (300 mL)
  5. washThe organic layer was washed successively with H2O and brine
  6. dry with materialAfter drying (Na2SO4)
  7. customthe solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-e536042bad33491cb5cec88fb0db431a
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08921350B2

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