HCID 59402271, Verbindung → HCID 59402254, Verbindung

HRID 2090483Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2090483
[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[CH:17]([CH3:18])[CH2:16][C:15]3[C:10](=[CH:11][C:12]([C:19]4[CH2:20][CH2:21][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:23][CH:24]=4)=[CH:13][CH:14]=3)[CH2:9]2)[CH:5]=[C:4]([N:32]2[CH2:37][CH2:36][N:35]([CH3:38])[CH2:34][CH2:33]2)[N:3]=1.[H][H]>CO.[Pd]>[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[CH:17]([CH3:18])[CH2:16][C:15]3[C:10](=[CH:11][C:12]([CH:19]4[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]([CH3:30])([CH3:31])[CH3:29])=[O:26])[CH2:21][CH2:20]4)=[CH:13][CH:14]=3)[CH2:9]2)[CH:5]=[C:4]([N:32]2[CH2:33][CH2:34][N:35]([CH3:38])[CH2:36][CH2:37]2)[N:3]=1

Komponenten

5

Edukt 2

HCID 59402271HCID 59402271, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 59402254HCID 59402254, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of tert-butyl 4-{2-[2-amino-6-(4-methylpiperazin-1-yl)pyrimidin-4-yl]-3-methyl-1,2,3,4-tetrahydroisoquinolin-7-yl}-3,6-dihydropyridine-1(2H)-carboxylate (Example 43, Step 1) (0.20 g, 0.38 mmol) in methanol (5 mL) was added palladium on carbon 10% wt. (20 mg) under an atmosphere of nitrogen. The mixture was vacuumed and re-charged with hydrogen three times, and stirred at r.t. for 48 h. The mixture was filtered. The filtrate was concentrated to afford the desired product which was directly used in next step reaction without further purification (200 mg, 99.61%). LCMS (M+H)+: m/z=522.3.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. concentrationThe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-37deef81a05e448696c9236bfd7ff743
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08436008B2

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