Trifluoroacetic acid → 3-Chloro-N-cyclopentyl-N-(3-hydroxy-propyl)-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate

HRID 2268632Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2268632
C(OC(=O)[N:7]([CH2:14][CH2:15][O:16][C:17]1[CH:22]=[C:21]([C:23](=[O:34])[N:24]([CH:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)[CH2:25][CH2:26][CH2:27][OH:28])[CH:20]=[C:19]([Cl:35])[CH:18]=1)[C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)(C)(C)C.[F:37][C:38]([F:43])([F:42])[C:39]([OH:41])=[O:40]>ClCCl>[F:37][C:38]([F:43])([F:42])[C:39]([OH:41])=[O:40].[Cl:35][C:19]1[CH:20]=[C:21]([CH:22]=[C:17]([O:16][CH2:15][CH2:14][NH:7][C:8]2[CH:9]=[CH:10][N:11]=[CH:12][CH:13]=2)[CH:18]=1)[C:23]([N:24]([CH:29]1[CH2:30][CH2:31][CH2:32][CH2:33]1)[CH2:25][CH2:26][CH2:27][OH:28])=[O:34]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 54299674(2-{3-Chloro-5-[cyclopentyl-(3-hydroxy-propyl)-carbamoyl]-phenoxy}-ethyl)-pyridin-4-yl-carbamic acid tert-butyl ester

Produkt 1

HCID 183492073-Chloro-N-cyclopentyl-N-(3-hydroxy-propyl)-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of (2-{3-chloro-5-[cyclopentyl-(3-hydroxy-propyl)-carbamoyl]-phenoxy}-ethyl)-pyridin-4-yl-carbamic acid tertbutyl ester (0.07 g) in a mixture of dichloromethane (2 ml) and trifluoroacetic acid (2 ml) was stored at room temperature for 1 h and then concentrated under reduced pressure. The residue was subjected to preparative hplc and the title compound (0.011 g) was obtained as a colourless gum by concentration of the required fraction under reduced pressure and drying by repetitive addition of acetonitrile and concentration under reduced pressure.

Aufarbeitung

  1. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4f09d7994ffb4dd6ac239e894e655839
Quelldatensatz
uspto-grants-2001_12
Patentnummer
US06326386B1

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