HCID 57786272, Verbindung → HCID 57786134, Verbindung

HRID 1399349Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1399349
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:14]2=[N:15][C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[C:17]=3[N:13]2[CH2:12][CH2:11][CH:10]=1>[Pd]>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]1[C:14]2=[N:15][C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[C:17]=3[N:13]2[CH2:12][CH2:11][CH2:10]1

Komponenten

3

Edukt 1

HCID 57786272HCID 57786272, Verbindung

Produkt 1

HCID 57786134HCID 57786134, VerbindungAusbeute 47 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23938PalladiumKatalysator

Versuchsvorschrift

A solution of 4-(2,4-dichlorophenyl)-N,N-diethyl-1,2-dihydropyrido[1,2-a]benzimidazol-9-amine (53.0 mg, 0.137 mmol) was stirred in the presence of 1.9% palladium on fibroin (10 mg) under hydrogen atmosphere at room temperature for 7 days. The catalyst was removed and the filtrate was concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with a 0-30% ethyl acetate/n-hexane gradient mixture to afford the desired product as pale yellow oil (24.8 mg, 0.0640 mmol, 47%).

Aufarbeitung

  1. customThe catalyst was removed
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was purified by column chromatography on silica gel eluting with a 0-30% ethyl acetate/n-hexane gradient mixture

Quellen und Nachweise

ORD-Eintrag
ord-75f0ffad68f34459a8987316dcc4b8cb
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08901141B2

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