HCID 21584328, Verbindung → HCID 21584267, Verbindung

HRID 583258Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 583258
[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-31dbfbf0d2d845288c6f33f8219b38a0
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05929085

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