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Ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate → HCID 18332960, Verbindung

HRID 2269722
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2269722
[N+:1]([C:4]1[CH:25]=[CH:24][CH:23]=[CH:22][C:5]=1[CH2:6][C:7]1([C:17](OCC)=[O:18])[CH2:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][CH3:15])[C:8]1=[O:16])([O-])=O>[C].[Pd].C(O)C>[O:16]=[C:8]1[C:7]2([CH2:6][C:5]3[C:4](=[CH:25][CH:24]=[CH:23][CH:22]=3)[NH:1][C:17]2=[O:18])[CH2:12][CH2:11][CH2:10][N:9]1[CH2:13][CH2:14][CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 18332952Ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate

Produkt 1

HCID 18332960HCID 18332960, VerbindungAusbeute 70,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

10% Palladium- carbon (0.2 g) was added to an ethanol solution (20 ml) of ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate (1.00 g), and catalytic hydrogenation was conducted at room temperature under one atmospheric pressure for 6 hours. The catalyst was removed by filtration and the filtrate was concentrated. The residue was dissolved in toluene (20 ml), which was heated under reflux for 12 hours. The reaction mixture was concentrated, and the obtained crude crystals were recrystallized from ethyl acetate-hexane to give the entitled compound (0.55 g).

Aufarbeitung

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in toluene (20 ml)
  4. temperaturewhich was heated
  5. temperatureunder reflux for 12 hours
  6. concentrationThe reaction mixture was concentrated
  7. customthe obtained crude crystals
  8. customwere recrystallized from ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-588de430343d40ec81df83959d8b1201
Quelldatensatz
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06329389B1

Notizen zur Reaktion

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