HCID 69422316, Verbindung → HCID 21073891, Verbindung

HRID 1373580Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1373580
[CH2:1]([C:3]1[N:8]=[C:7]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][CH:18]=[CH:19][C:20]3[N:29]=[C:28]4[C:23]([CH2:24][CH2:25][C:26](=[O:30])[NH:27]4)=[CH:22][CH:21]=3)[CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1)[CH3:2]>CCO.[Pd]>[CH2:1]([C:3]1[N:8]=[C:7]([N:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]3[N:29]=[C:28]4[C:23]([CH2:24][CH2:25][C:26](=[O:30])[NH:27]4)=[CH:22][CH:21]=3)[CH2:13][CH2:14]2)[CH:6]=[CH:5][CH:4]=1)[CH3:2]

Komponenten

4

Edukt 1

HCID 69422316HCID 69422316, Verbindung

Produkt 1

HCID 21073891HCID 21073891, VerbindungAusbeute 10 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

7-{5-[4-(6-Ethyl-pyridin-2-yl)-piperazin-1-yl]-pent-1-enyl}-3,4-dihydro-1H-[1,8]naphthyridin-2-one (0.515 g, 1.27 mmol) was hydrogenated using 20% Pd/C in EtOH for 103 h. The reaction was filtered and concentrated. Purification by liquid chromatography (Biotage 12 SiO2 column, CH2Cl2 to 1% MeOH/CH2Cl2) followed by recrystallization from Et2O gave the title compound as a solid (50 mg, 0.012 mmol, 10%). MS: APCI: M+1: 408.2 (Exact Mass: 407.27).

Aufarbeitung

  1. customfor 103 h
  2. filtrationThe reaction was filtered
  3. concentrationconcentrated
  4. customPurification by liquid chromatography (Biotage 12 SiO2 column, CH2Cl2 to 1% MeOH/CH2Cl2)
  5. customfollowed by recrystallization from Et2O

Quellen und Nachweise

ORD-Eintrag
ord-824fbef95a2745dc8472805b74da12ca
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07160888B2

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