(1-Nitromethylcyclohexyl)acetic acid ethyl ester → 2-Azaspiro(4.5)decan-3-one

HRID 1535025Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1535025
[N+:1]([CH2:4][C:5]1([CH2:11][C:12]([O:14]CC)=O)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)([O-])=O>C(O)C.[C].[Pd]>[CH2:4]1[C:5]2([CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]2)[CH2:11][C:12](=[O:14])[NH:1]1

Komponenten

4

Edukt 1

HCID 11128083(1-Nitromethylcyclohexyl)acetic acid ethyl ester

Produkt 1

HCID 474572-Azaspiro(4.5)decan-3-oneAusbeute 91,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

190 g (0 82 mole) Ethyl 1-nitromethyl-1-cyclohexaneacetate in 3168 mL ethanol are hydrogenated for 4 hours at 125° C. in the presence of 62.9 g 10% palladium-carbon. At the end of the take up of hydrogen, the catalyst is filtered off and the colorless solution obtained is distilled to dryness in a vacuum. 116.2 g 2-Aza-spiro[4,5]decan-3-one in the form of a colorless crystallizate are obtained; yield 91.6% of theory. Content 97.1% (GC); m.p. 88° to 90° C.

Aufarbeitung

  1. filtrationAt the end of the take up of hydrogen, the catalyst is filtered off
  2. customthe colorless solution obtained
  3. distillationis distilled to dryness in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-d7134c37bf914407a9e8e97cdc5b727c
Quelldatensatz
uspto-grants-1992_02
Patentnummer
US05091567

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