4-Benzyloxy-1-{2-oxo-2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one → 4-Hydroxy-1-{2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one

HRID 564084

Reaktionsgleichung

C([O:8][C:9]1[CH:14]=[CH:13][N:12]([CH2:15][C:16](=O)[C:17]2[CH:33]=[CH:32][C:20]3[CH2:21][CH2:22][N:23]([C:26](=[O:31])[C:27]([F:30])([F:29])[F:28])[CH2:24][CH2:25][C:19]=3[CH:18]=2)[C:11](=[O:35])[CH:10]=1)C1C=CC=CC=1>CO.Cl.[Pd]>[OH:8][C:9]1[CH:14]=[CH:13][N:12]([CH2:15][CH2:16][C:17]2[CH:33]=[CH:32][C:20]3[CH2:21][CH2:22][N:23]([C:26](=[O:31])[C:27]([F:28])([F:29])[F:30])[CH2:24][CH2:25][C:19]=3[CH:18]=2)[C:11](=[O:35])[CH:10]=1

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

To 5.00 g (10.3 mmol) 4-benzyloxy-1-{2-oxo-2-[3-(2,2,2-trifluoro-acetyl)-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl]-ethyl}-1H-pyridin-2-one (preparation 21a) in 100 mL MeOH and 9.8 mL 1 M aqueous HCl-solution is added 500 mg of 10% Pd/C. The reaction mixture is stirred under a hydrogen atmosphere of 5000 hPa at 50° C. for 18 h. After filtration and evaporation of the solvent, is the residue purified by HPLC (Zorbax stable bond, C18; water (0.15% formic acid)/acetonitrile 95:5 to 5:95).

Aufarbeitung

filtrationAfter filtration and evaporation of the solvent
custompurified by HPLC (Zorbax stable bond, C18; water (0.15% formic acid)/acetonitrile 95:5 to 5:95)

Quellen und Nachweise

ORD-Eintrag: ord-e646eb6962724d7cb52170bde82d6f38
Quelldatensatz: uspto-grants-2011_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08067590B2

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