Hydrochloric Acid → 1-Ethylcarbonyl-4-oxohomopiperidine

HRID 556914Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 556914
[O:1]=[C:2]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.Cl.[C:10]([O-:13])([O-])=O.[K+].[K+].ClC(O[CH2:20][CH3:21])=O>C1COCC1>[CH2:20]([C:10]([N:5]1[CH2:6][CH2:7][CH2:8][C:2](=[O:1])[CH2:3][CH2:4]1)=[O:13])[CH3:21]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 1501891Azepan-4-one

Produkt 1

HCID 186757361-Ethylcarbonyl-4-oxohomopiperidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a cold (0° C.) stirred solution of 4-oxohomopiperidine.HCl (0.6 g, 4.05 mmol), K2CO3 (0.615 g, 4.46 mmol) in anhydrous THF (10 mL) will be ethyl chloroformate (0.44 mL, 4.05 mmol) dropwise. The reaction was warmed to RT for 2 hrs then quenched with H2O, extracted with EtOAc, and the organic layer dried over Na2SO4. Pure 1-ethylcarbonyl-4-oxohomopiperidine will be isolated via silica gel flash chromatography

Aufarbeitung

  1. customthen quenched with H2O
  2. extractionextracted with EtOAc
  3. dry with materialthe organic layer dried over Na2SO4

Quellen und Nachweise

ORD-Eintrag
ord-1c714051aeff4d14845e05cf1553425d
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08058287B2

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