HCID 67429355, Verbindung → HCID 86625703, Verbindung

HRID 1662669Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1662669
C(OC(=O)[N:10]([CH2:18][CH2:19][O:20]CC1C=CC=CC=1)[C@@H:11]([CH3:17])[C:12]([N:14]([CH3:16])[CH3:15])=[O:13])C1C=CC=CC=1.[H][H]>CCO.[Pd]>[OH:20][CH2:19][CH2:18][NH:10][C@@H:11]([CH3:17])[C:12]([N:14]([CH3:16])[CH3:15])=[O:13]

Komponenten

5

Edukt 2

HCID 67429355HCID 67429355, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 86625703HCID 86625703, VerbindungAusbeute 64,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

Under nitrogen atmosphere, to a solution of 2.75 g of the compound obtained in Step 79-2 in EtOH (30 ml) was added palladium-activated carbon (10% Pd, 0.30 g), and the inside of the reaction system was displaced with hydrogen gas. The solution was stirred for 24 hours at 45° C., then, the reaction solution was filtered, and the solvent was filtered out under reduced pressure. To a solution of the obtained residue in EtOH (30 ml) solution was added palladium-activated carbon (10% Pd, 0.30 g), and the reaction system was displaced with hydrogen gas, again. The solution was stirred for one day at 45° C., then, the reaction solution was filtered, and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60; mobile phase: CHCl3/MeOH=9/1 to 4/1; v/v) to obtain 734 mg of the title compound (colorless oil).

Aufarbeitung

  1. filtrationthe reaction solution was filtered
  2. filtrationthe solvent was filtered out under reduced pressure
  3. additionTo a solution of the obtained residue in EtOH (30 ml) solution was added palladium-activated carbon (10% Pd, 0.30 g)
  4. stirringThe solution was stirred for one day at 45° C.
  5. filtrationthe reaction solution was filtered
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by column chromatography (silicagel 60; mobile phase: CHCl3/MeOH=9/1 to 4/1; v/v)

Quellen und Nachweise

ORD-Eintrag
ord-36421ef84bcf4397a2eca8bf46779876
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08030499B2

Notizen zur Reaktion

Wird geladen…