HCID 21584328, Verbindung → HCID 21584267, Verbindung

HRID 369958Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 369958
[ClH:1].[N+:2]([C:5]1[CH:18]=[CH:17][C:8]2[CH2:9][CH:10]3[N:15]([CH2:16][C:7]=2[CH:6]=1)[CH2:14][CH2:13][CH2:12][CH2:11]3)([O-])=O>C(O)C.[Pd]>[ClH:1].[CH2:11]1[CH:10]2[N:15]([CH2:16][C:7]3[CH:6]=[C:5]([NH2:2])[CH:18]=[CH:17][C:8]=3[CH2:9]2)[CH2:14][CH2:13][CH2:12]1

Komponenten

4

Edukt 1

HCID 21584328HCID 21584328, Verbindung

Produkt 1

HCID 21584267HCID 21584267, VerbindungAusbeute 95,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

8-Nitro-1,3,4,6,11,11a-hexahydro-2H-benzo[b]quinolizine hydrochloride (2.93 g, 10.9 mmol) was dissolved in ethanol (150 ml) and 10% palladium-on-carbon (0.4 g) was added and the solution was shaken on a Parr Hydrogenator for 2 h. The catalyst was filtered off and the catalyst was washed with water. The filtrate was concentrated and absolute ethanol was added and evaporated to drive off excess water. The resulting solid was taken up in hot ethanol (75 ml) and ether (100 ml) was added slowly. The precipitate which formed was collected and dried in the air to give the title compound as an off-white solid (2.48 g, 95%), m.p. 241-3° C. (dec.).

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. washthe catalyst was washed with water
  3. concentrationThe filtrate was concentrated
  4. additionabsolute ethanol was added
  5. customevaporated
  6. additionether (100 ml) was added slowly
  7. customThe precipitate which formed
  8. customwas collected
  9. customdried in the air

Quellen und Nachweise

ORD-Eintrag
ord-c9a5ceb6f3464edb98a166c30b715df4
Quelldatensatz
uspto-grants-2000_10
Patentnummer
US06140322

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